Chlorides-buliding-blocks

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., name: 1-Bromo-3,5-dichlorobenzene

In the environment of nitrogen dissolved in I-20(85 g, 179 mmol) 700 mL of tetrahydrofuran (THF), where the 1-bromo-3,5-dichlorobenzene(48.5 g, 215 mmol) and tetrakis( triphenylphosphine) palladium was stirred into the (2.07 g, 1.79 mmol).Into a saturated potassium carbonate in water (61.8 g, 448 mmol) was heated to reflux at 80 ° C for 7 hours. After the reaction was completed, the reaction solution into water and extracted with dichloromethane (DCM) and then water was removed with anhydrous MgSO4, filter and was concentrated under reduced pressure. Thus separated and purified theresulting residue was purified by flash column chromatography compound to obtain a I-21(72.6 g, 82percent)

According to the analysis of related databases, 19752-55-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Cheil Industries Co., Ltd; Lee, Han Ir; Yu, Uhn Sun; Kang, Dong Min; Kang, Uii Soo; Yang, Yong Tak; Oh, Jae Jin; Yu, Dong Gyu; Lee, Sang Sin; Jang, Yuna; Jung, Su Young; Han, Su Jin; Hong, Jin Suk; (59 pag.)KR2015/6758; (2015); A;,
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Adding a certain compound to certain chemical reactions, such as: 13078-80-3, name is 2-(2-Chlorophenyl)ethanamine, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 13078-80-3, Quality Control of 2-(2-Chlorophenyl)ethanamine

N-(2-Fluoropyrimidin-4-yl)-N-methyl-2-phenylpyrimidin-4-amine (442 mg, 1.5 mmol), 2-(2-chlorophenyl)ethanamine (0.32 mL, 2.25 mmol), and dioxane (7 mL) were mixed in a 25 mL roundbottom flask. The mixture was stirred at 100 C. overnight under nitrogen. The reaction was concentrated by vacuum and quenched with saturated NaHCO3 solution. The white solid was filtered and recrystallized to give N2-(2-chlorophenethyl)-N4-methyl-N4-(2-phenylpyrimidin-4-yl)pyrimidine-2,4-diamine as a white solid. MS m/z 417 (MH)+.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 2-(2-Chlorophenyl)ethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Andersen, Denise Lyn; Chang, Catherine H.; Falsey, James R.; Frohn, Michael J.; Hong, Fang-Tsao; Liao, Hongyu; Liu, Longbin; Lopez, Patricia; Retz, Daniel Martin; Rishton, Gilbert M.; Rzasa, Robert M.; Siegmund, Aaron; Tadesse, Seifu; Tamayo, Nuria; Tegley, Christopher M.; US2006/69110; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 445-13-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 445-13-6 as follows.

General procedure: A substituted aniline (3.0 mmol) and CDI (3.0 mmol) were dissolvedin anhydrous dichloromethane (15 mL) and the reaction was stirred atroom temperature for 1 h under a nitrogen atmosphere. The solvent wasthen removed under reduced pressure, yielding the crude carbamoylimidazolesas solids. The carbamoylimidazoles were then dissolved indichloromethane (5 mL), and added to a solution of amine 13a or 13b(2.0 mmol) in dichloromethane (15 mL). The reaction was then left tostir for 1 h at room temperature. Dichloromethane (50 mL) was thenadded, and the organic layer was washed with water (3×100 mL). Theorganic layer was dried over Na2SO4 and concentrated under reducedpressure. The product was purified on silica gel by step-wise gradientelution with dichloromethane/ethyl acetate (100:0 to 90:10).

According to the analysis of related databases, 445-13-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Al-Zubaidi, Yassir; Pazderka, Curtis; Koolaji, Nooshin; Rahman, Md Khalilur; Choucair, Hassan; Umashankar, Bala; Bourget, Kirsi; Chen, Yongjuan; Rawling, Tristan; Murray, Michael; European Journal of Pharmaceutical Sciences; vol. 129; (2019); p. 87 – 98;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3-Chloropropan-1-amine hydrochloride

3-Chloropropylamine hydrochloride (12 mg, 0.093 mmol), 1-(3-dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (EDC, 17 mg, 0.089 mmol), 4,4-dimethylaminopyridine (DMAP, 1 mg 0.008 mmol) and Et3N (50 muL, 0.359 mmol) were added to a solution of 1-pyreneacetic acid (20 mg, 0.077 mmol) in anhydrous CH2Cl2 (1 mL) under an argon atmosphere. The reaction mixture was stirred at room temperature for 7 h, quenched with aqueous saturated NH4Cl solution, and extracted with AcOEt. The organic layer was washed with brine, dried over Na2SO4 and evaporated in vacuo. The resulting residue was purified by silica gel column chromatography (CH2Cl2) to give 6 as a pale yellow solid (13 mg, 50%). 1H-NMR (400 MHz, CDCl3) delta (ppm) 8.20 (2H, d, J = 7.6 Hz), 8.15 (3H, d, J = 7.9 Hz), 8.08 (1H, d, J = 9.2 Hz), 8.04 (1H, d, J = 9.2 Hz), 8.02 (1H, t, J = 7.9 Hz), 7.88 (1H, d, J = 7.9 Hz), 4.28 (2H, s), 3.31 (2H, t, J = 6.4 Hz), 3.25 (2H, q, J = 6.4 Hz), 1.78 (2H, quin, J = 6.4 Hz). 13C-NMR (125 MHz, CDCl3) delta (ppm) 171.23, 131.28, 131.16, 130.76, 129.53, 128.50, 128.16, 127.69, 127.27, 126.28, 125.60, 125.48, 125.20, 125.12, 124.62, 122.76, 42.22, 42.08, 37.28, 31.86. IR (cm-1): 3293, 1646, 1544. HR ESI-MS (m/z): calcd. for [C21H19ClNO]+, 336.1150 ([M+H]+); found 336.1161.

The synthetic route of 6276-54-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Fuchi, Yasufumi; Obayashi, Hideto; Sasaki, Shigeki; Molecules; vol. 20; 1; (2015); p. 1078 – 1087;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 363-51-9, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 363-51-9 as follows.

EXAMPLE 7 (1H-Benzimidazol-2-yl)-(2-chloro-6-fluorophenyl)amine hydrochloride 2-Chloro-6-fluoroaniline (0.48 g) and 2-chlorobenzimidazole (0.5 g) were mixed in a flask and then kept at 170 C. for 30 min. After cooling, the residue was dissolved out of the flask at boiling heat using 1 N HCl and 10% ethanol. The material dissolved out was then stirred at RT for 30 min, then the insoluble material was filtered off with suction and the filtrate was evaporated. The residue was purified by means of preparative HPLC on RP-18 using acetonitrile/water (0.05% TFA). The clean fractions were combined, the acetonitrile was stripped off, the residue was adjusted to pH 10 with potassium carbonate solution, extracted three times with EA, and then the combined phases were dried, filtered, and concentrated. The residue was taken up using HCl/water and freeze-dried. 27 mg of the title compound were obtained. LCMS-Rt: 3.45 min; MS (ES+, M+H+): 262.0

According to the analysis of related databases, 363-51-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hofmeister, Armin; Heinelt, Uwe; Lang, Hans-Jochen; Bleich, Markus; Wirth, Klaus; Gekle, Michael; US2002/132842; (2002); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 202197-26-0, A common heterocyclic compound, 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline, molecular formula is C13H11ClFNO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: To a 50-ml glass round-bottom flask was added sequentially the primary amine 2 (1.0 mmol; aliphatic, aromatic or heteroaromatic; as free naked amine or as HCl, MsOH, TsOH or tartrate salt), FSO2N3 solution (containing 1.0 mmol FSO2N3, approximately 200 mM in DMF/MTBE 1:1, v/v, approximately 5 ml, volume adjusted according to the concentration; prepared according to the above procedure and diluted with equal volume of DMF) and aqueous KHCO3 solution (3.0 M, 1.33 ml, containing 4.0 mmol KHCO3). The reaction mixture was stirred for 5 min at room temperature, while monitoring by LC-MS. After completion, EtOAc (40 ml) was added and the mixture was washed sequentially with brine (60 ml × 6), water (60 ml × 2) and brine (60 ml), dried over Na2SO4, concentrated by rotary evaporation and dried under vacuum to afford the azide product 3. For products containing acidic functional groups, this extraction process was modified with acidified aqueous phase (acidified with aqueous HCl). Detailed procedures and the various modifications, as well as the characterization data for each compound, can be found in Supplementary Information 1.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Meng, Genyi; Guo, Taijie; Ma, Tiancheng; Zhang, Jiong; Shen, Yucheng; Sharpless, Karl Barry; Dong, Jiajia; Nature; vol. 574; 7776; (2019); p. 86 – 89;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 81927-55-1 as follows. Application In Synthesis of Benzyl 2,2,2-trichloroacetimidate

To a solution of scheme 58 compound Si (24 g, 0136 mol) and benzyl 2,2,2- thchioroaceiirnidate (5 1)3 g, 0204 inol) in cvchexanedichloromethane (600 inL120 ml..) at room temperature was added tritluorornethanesulfonic anhydride (cat. 1 .2 mE) dropwise. The reaction mixture was stirred at room temperature overnight and filtered. The filtrate was washed 4lth sat N& K (Y and hnne, dned o ci anh chous Na2SO- filteted and ctncentiated he residue was purified by column chromatography on silica gel (eluted with petroleum ether: ethyl aceiate =10: 1) to give the title compound (35 g, 933% yield) as a yellow oil.

According to the analysis of related databases, 81927-55-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WILES, Jason Allan; PHADKE, Avinash S.; DESHPANDE, Milind; AGARWAL, Atul; CHEN, Dawei; GADHACHANDA, Venkat Rao; HASHIMOTO, Akihiro; PAIS, Godwin; WANG, Qiuping; WANG, Xiangzhu; GREENLEE, William; (358 pag.)WO2017/35411; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 1205-71-6, name is 4-Chloro-N-phenylaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C12H10ClN

In a 250ml round bottom flask,10-bromobenzo [b] naphtho [2,1-d] furan (12 mmol), copper iodide (15 mmol), potassium tert-butoxide (65 mmol),1,2-diaminocyclohexane (12 mmol)And (4-chloro-phenyl) -phenylamine (12 mmol) were added to dry 1,4-dioxane (100 ml) and refluxed for 48 hours under N2 atmosphere. The obtained intermediate was cooled to room temperature, and added Water was then filtered through a pad of diatomaceous earth while being extracted with dichloromethane, then washed with water, and dried over anhydrous magnesium sulfate. After filtration and evaporation, the crude product was purified by silica gel column chromatography to obtain the intermediate HT002-1.

The synthetic route of 1205-71-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Tianma Organic Shine Display Co., Ltd.; Zhang Lei; Gao Wei; Niu Jinghua; Dai Wenpeng; Xiao Wenjing; Lu Yan; Zhu Hongyan; (28 pag.)CN110746391; (2020); A;,
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Chlorides – an overview | ScienceDirect Topics

Application of 1996-29-8,Some common heterocyclic compound, 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, molecular formula is C6H3BrClF, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Under a nitrogen atmosphere, 104.7 g of 2-fluoro-4-chlorobromobenzene, 400 ml of THF and 67.3 g of potassium t-butoxide were added to a 1 L three-necked flask.After cooling to -60 C, 300 mL of n-butyl lithium solution (2 mol / L) was added dropwise, and the addition was completed -50 to -60 CAfter heat preservation for 1 h, the temperature was raised to -30 C, and then 172.6 g of tributyl borate was added dropwise.After the completion of the dropwise addition, the temperature was naturally raised to room temperature for 2 hours.The reaction solution is acidified with hydrochloric acid, extracted with petroleum ether, and washed with water.Concentrated to a white solid a-1, 75.1 g, Y = 86.1%,LC = 98.15%. 2) Synthesis of a-2: under nitrogen protection,Add a-1 41.9g to a 250ml three-necked bottle.4-bromo resorcinol37.8g, potassium carbonate 27.6g,TBAB 2.0g, Pd(0) 0.5g, ethanol 100mL, water 50mL,After stirring at reflux for 3 h, the reaction solution was acidified with dilute hydrochloric acid.Extracted with ethyl acetate and concentrated.Recrystallization from 2 times ethanol gave a white solid a-2.38.5 g, Y = 80.7%, GC = 98.78%. 3) Synthesis of a-3: under nitrogen protection,Add a-223.9g to a 100ml three-necked bottle.DMF 70mL, 60% sodium hydride 8.0g,Reflow reaction for 0.5 h,The reaction solution was poured into ice water, neutralized with dilute hydrochloric acid, and extracted with ethyl acetate, and evaporated to give a yellow solid a-3, 20.9 g,GC=98.61% 4) Synthesis of a-4: A-320.9 g was sequentially added to a 100 ml three-necked flask.60 mL of dichloromethane,21.7 g of trimethylchlorosilane, reacted at room temperature for 0.5 h, concentrated,A yellow solid a-4, 27.8 g, Y = 100%, GC = 98.65%. 5) Synthesis of a-5: under nitrogen protection,Add a-423.3g to a 250 mL three-necked flask.THF 100ml, potassium t-butoxide 10.8g, after cooling to -50 C,60 mL of n-butyllithium solution (2 mol/L) was added dropwise.After the addition is completed, the temperature is kept at -50 to -40 C for 1 h.After heating to -30 C, 27.6 g of tributyl borate was added dropwise.After the completion of the dropwise addition, the temperature was naturally raised to room temperature for 2 hours. The reaction mixture was acidified with hydrochloric acid, extracted with EtOAc EtOAc.Y = 74.2%, LC = 98.66%. 6) Synthesis of a-6: Under nitrogen protection, 4-bromo resorcinol 9.5 g, a-5 17.8 g, potassium carbonate 13.8 g, TBAB 1.0 g were sequentially added to a 100 ml three-necked flask.Pd(0)0.2g, ethanol 50mL, water 20mL, reflux and stirring for 5h,The reaction solution was acidified with dilute hydrochloric acid, extracted with toluene, and concentrated.Recrystallization from 2 times ethanol gave a pale yellow solid a-6.13.1 g, Y = 71.9%, GC = 99.18%. 7) Synthesis of a-7: A-6 10.9 g was added to a 100 ml three-necked bottle in turn.50mL of dichloromethane, 9.4g of tetrabutylammonium fluoride,The reaction was refluxed for 1 h, washed with water and concentrated to give a pale yellow solid a-7.8.1 g, Y = 92.0%, LC = 98.76%. 8) Synthesis of a: under nitrogen protection,Add a-75.8g to a 100ml three-necked bottle.50 mL of dichloromethane and 9.1 g of triethylamine.The polymerization inhibitor is 0.01 g of hydroquinone, and a mixed solution of 7.5 g of methacryloyl chloride and 15 mL of dichloromethane is added dropwise in an ice water bath, and the mixture is naturally added to room temperature and stirred for 0.5 h after the dropwise addition.The reaction solution is acidified with dilute hydrochloric acid, washed with water and concentrated.Recrystallization from 1x ethanol and 2 times n-heptane mixed solvent,Purified by silica gel column to obtain product a, 5.2g, Y=52.5%,LC = 99.90%.

The synthetic route of 1996-29-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xi’an Ruili Electronic Materials Co., Ltd.; Li Chao; Zhao Wen; Zhang Yanli; Jin Linuo; (35 pag.)CN109503534; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 50638-47-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 50638-47-6, name is 4-Bromo-2-chloro-1-methoxybenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a magnetically stirring solution of 4-bromo-2-chloroanisole (0.50 g, 2.61 mmol) and 1- CYCLOPENTYL-2-PROPEN-1-OL (1.5 eq, 0.49 g, 3.88 mmol) in anhydrous N-methylpyrrolidinone (3.0 mL), under argon at room temperature, was added sodium bicarbonate (1.2 eq, 0.26 g, 3.10 mmol) followed by DICHLOROBIS (TRIPHENYLPHOSPHINE) PALLADIUM (II) (0.02 eq, 36.7 mg, 0.05 MMOL). The resulting mixture was heated to 140 C in an oil bath and maintained for 4 hours. The resulting dark reaction mixture was cooled to room temperature and poured into water (50 mL) and extracted with EtOAc (2 X 25 mL). The organics were washed with water (50 mL) and brine (50 mL) then dried over NA2SO4, filtered and concentrated. The crude residue was purified by flash chromatography (1% through 10% EtOAc in Hexanes) to yield the intermediate ketone as a slightly yellow oil (0.49 g, 79%).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Bromo-2-chloro-1-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PFIZER INC.; WO2004/74270; (2004); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics