Category: chlorides-buliding-blocks

Related Products of 15205-15-9, These common heterocyclic compound, 15205-15-9, name is 2-Chloro-6-fluorobenzylamine, 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: A mixture of 0.55mmol of 8-bromo-7-(2-bromoethyl)theophylline 7a or 8-bromo-7-(3-chloropropyl)theophylline 7b or 8-bromo-7-(4-bromobutyl)theophylline 7c, 1.1mmol of appropriate aromatic amine, 1,6 mmol of TEBA and 1.00ml of propanol was heated in closed vessels in microwave oven (300 Watt, Power Max Off, 160C, 10bar) for 1h. The solvent was removed and the residue was treated with ethanol. The products were purified by crystallization from ethanol or flash column chromatography over silica gel with CH2Cl2 : MeOH (100 : 0 to 80 : 20). The precipitate was filtered off and dried.

The synthetic route of 15205-15-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Za?uski, Micha?; Schabikowski, Jakub; Schlenk, Miriam; Olejarz-Maciej, Agnieszka; Kubas, Bart?omiej; Karcz, Tadeusz; Kuder, Kamil; Latacz, Gniewomir; Zygmunt, Ma?gorzata; Synak, David; Hinz, Sonja; Mueller, Christa E.; Kie?-Kononowicz, Katarzyna; Bioorganic and Medicinal Chemistry; vol. 27; 7; (2019); p. 1195 – 1210;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline, A new synthetic method of this compound is introduced below., COA of Formula: C13H11ClFNO

General procedure: Acetic acid (2.0 mL) and aniline derivatives (1.10mmol) was added to 6 (1.00 mmol). The mixturewas heated to 125-130 C andstirred for 15 min. The reaction mixture was then cooled to 25 C.The acetic acid was evaporated. To the reaction mixture, ice-water(10 mL) was added and adjusted pH to 9 with ammonium hydroxide.The mixture was stirred for 0.5 h. The precipitated productwas filtered, and the filtered cake was washed with water(3 x 10 mL) to afford crude product. The crude product was chromatographedby silica gel, eluting with EtOAc/petroleum ether(1:4) to afford 7a-7f (yield 82-94%) as white solid. 4.1.7.1 4-(3-chloro-4-(3-fluorobenzyloxy)phenylamino)-6,7-bis(2-chloroethoxy)quinazoline (7a) Yield: 86%. 1H NMR (600?MHz, DMSO-d6) delta(ppm): 9.47 (s, 1H), 8.48 (s, 1H), 7.97 (d, J?=?2.6?Hz, 1H), 7.91 (s, 1H), 7.71 (dd, J?=?8.9, 2.6?Hz, 1H), 7.50-7.46 (m, 1H), 7.35-7.31 (m, 2H), 7.28 (s, 1H), 7.26 (s, 1H), 7.20-7.16 (m, 1H), 5.25 (s, 2H), 4.48-4.45 (m, 4H), 4.08 (t, J?=?5.5?Hz, 2H), 4.04 (t, J?=?5.0?Hz, 2H). 13C NMR (151?MHz, DMSO-d6) delta(ppm): 162.2 (d, 1JC-F?=?243.7?Hz), 156.3, 153.2, 153.1, 149.5, 147.5, 147.0, 139.7, 139.6, 133.4, 130.5 (d, 3JC-F?=?8.3?Hz), 124.0, 123.3 (d, 4JC-F?=?2.6?Hz), 122.1, 121.1, 114.6 (d, 2JC-F?=?20.9?Hz), 114.3, 114.0 (d, 2JC-F?=?21.9?Hz), 109.0 (d, 3JC-F?=?8.6?Hz), 104.7, 69.5, 69.4, 68.9, 42.7, 42.6.

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; Zhang, Yaling; Chen, Li; Xu, Hongjiang; Li, Xiabing; Zhao, Lijun; Wang, Wei; Li, Baolin; Zhang, Xiquan; European Journal of Medicinal Chemistry; vol. 147; (2018); p. 77 – 89;,
Chloride – Wikipedia,
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Related Products of 261762-56-5, 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 261762-56-5 as follows.

In a four-necked 250 mL round-bottomed flask, equipped with a thermometer, a reflux condenser with pressure equalizer, a dry ice cooled dropping funnel (-30 C) and a gas inlet, 50.0 g (purity 97.0 w%, 302 mmol, 1.0 eq) of l-chloro-2-fluoro-3-methoxy-benzene (1, CAS- No. 261762-56-5) were dissolved in 70 mL of chlorobenzene. To the solution 53.1 g (purity 98.0 w%, 332 mmol, 1.1 eq) bromine was added over one hour at 5-10 C internal temperature via cooling externally at 0 C. After complete addition the reaction was allowed to reach 25 C. The reaction was continued for further 8 hours under a constant stream of nitrogen purge gas to remove HBr from the reaction mixture. Afterwards a HPLC measurement indicated >98% conversion. The reaction solution was then washed with 100 mL of aqueous saturated NaHC03 solution and 50 mL of deionized water. Afterwards the organic phase was dried over MgSC^, the drying agent was filtered off and the solvent was removed in vacuum at 65 C and 5 mbar to leave 72.6 g (90%, purity 90%) of a brownish solid. The solid was purified via vacuum distillation at 10 mbar and temperature of 118-122 C to yield 57.4 g (79%, purity 99%) of a white solid. NMR (CDC13, 400 MHz) delta (ppm) = 7.34 (dd, J= 8.0, 2.0 Hz, 1H), 6.79 (dd, J= 8.0, 8.0 Hz, 1H), 3.89 (s, 3H).

According to the analysis of related databases, 261762-56-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; MUeHLTHAU, Friedrich, August; FORD, Mark, James; ERVER, Florian; BREMEYER, Nadine; PLATZEK, Johannes; GUIMOND, Nicolas; BADER, Thomas; ALBRECHT, Uwe; (129 pag.)WO2018/46684; (2018); 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. 38762-41-3, name is 4-Bromo-2-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 4-Bromo-2-chloroaniline

General procedure: Phenyl phenylphosphoramidochloridate (1) (0.001 mol) and 2-amino-benzothiazole (2a) (0.001 mol) were taken in a bottomed flask (50 mL) and THF (20 mL) was added. To thismixture, dimethylpiperazine (DMP) (0.001 mol) was added andthe reaction mixture was stirred vigorously at 30-50 C for 4 h.The progress of the reaction was monitored by TLC. After completionof the reaction, DMP. HCl was removed by filtration andthe filtrate was concentrated under vacuum and the resultantsolidwas purified by passing through a columnof silica gel usinghexane:ethyl acetate (2:1) as an eluent to afford title compound,phenylN-1,3-benzothiazol-2-yl-N?-phenylphosphorodiamidate(3a). The same experimental procedure was adopted for the preparation of the remaining title compounds (3b-j) (Scheme 1).

The synthetic route of 38762-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Nayab Rasool; Babu, P. Hari; Janaki Ramudu; Jyothi Kumar; Appa Rao, Ch.; Raju, C. Naga; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 193; 1; (2018); p. 10 – 13;,
Chloride – Wikipedia,
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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., SDS of cas: 19752-55-7

To a solution of 1-bromo-3,5-dichlorobenzene (25.0 g, 1 10.6 mmol) in 400 ml THF at room temperature, isopropyl magnesium chloride lithium chloride complex (85.0 ml, 1.3M THF, 1 10.6 mmol) was added dropwise at room temperature over a period of 15 minutes while holding the reaction temperature between 20°C and 25°C. After the addition was complete, the reaction was allowed to stir 1.5 hours at room temperature. The reaction solution was then cooled to -5 °C to -10 °C with ice/MeOH. Methyltrifluoroacetate (12.23 ml, 121 .6 mmol) in 20 ml THF was added dropwise to the reaction solution while maintaining the reaction temp below 0 °C (~ 30 min). The reaction was stirred at -5 °C for 0.5 hr then was allowed to warm to room temperature and stir for 1.5 hrs. The reaction was cooled again to -5 °C to -10 °C then 73.7 ml 6M HCI diluted to 150 ml total volume water was added dropwise while keeping the temperature below 0 °C. Once the addition was complete, the reaction was stirred 0.5 hr at 0 °C then was allowed to warm to room temperature. Excess water was added and the resulting organic layer that separated was drawn off. The aqueous layer was washed repeatedly with DCM. The combined DCM washes and recovered organic layer were dried over sodium sulfate and concentrated to yield 90 g of an oil. The crude material was then passed through a silica gel plug (neat heptane to neat DCM) and purified by vacuum distillation (3 torr, product fractions recovered froml 12 °C to 125 °C) to provide 20.3 g product (75.7percent yield). 1 H NMR (400 MHz, CHLOROFORM-d) delta ppm 7.71 (s, 1 H) 7.93 (s, 2 H). IR 1728.1 cm”1

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 19752-55-7.

Reference:
Patent; AVISTA PHARMA SOLUTIONS, INC.; SPEAKE, Jason, D.; (57 pag.)WO2018/9751; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 433-94-3, These common heterocyclic compound, 433-94-3, name is 2-Chloro-6-(trifluoromethyl)aniline, 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.

Preparation 9 2-Chloro-6-trifluoromethyl-phenyl)-hvdrazine hydrochlorideTo a 0 0C solution of 2-chloro-6-trifluoromethyl-phenylamine (35.7 mmol, 7.0 g) in THF (100 mL) is added 48% BF3OEt (143 mmol, 36 mL) followed by addition of isoamyl nitrite (143 mmol, 19 mL). The reaction is stirred for 1 hour and is filtered to collect the tetrafluoroborate diazonium salt (48.7 mmol, 9.0 g). The salt is dissolved in a mixture of cone. HCl (30 mL) and water (10 mL) at 0 0C. To the resulting mixture is added ascorbic acid (48.7 mmol, 8.5 g). The reaction is heated to 50 0C for 3 hours and cooled to room temperature. The solid is filtered and washed with ice water. The wet solid is dissolved in a mixture of cone. HCl (30 mL) and water (20 mL) and heated to 90 0C for 2 hours. The reaction is cooled to 0 0C and filtered to yield the title compound (5.0 g, 60%). LC-ES/MS m/e 157.0 (M+l).

The synthetic route of 433-94-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2007/140183; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 39885-50-2,Some common heterocyclic compound, 39885-50-2, name is 2-Chloro-4-(trifluoromethyl)aniline, molecular formula is C7H5ClF3N, 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.

5-Amino-1-(2-chloro-4-trifluoromethylphenyl)-3-cyanopyrazole in the form of an orange crystalline solid, m.p. 133°-135° C., from 2-chloro-4-trifluoromethylaniline. 5-Amino-3-cyano-1-(2,4,6-trichlorophenyl)pyrazole in the form of a light brown solid, m.p. 155-156° C., from 2,4,6-trichloroaniline.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-4-(trifluoromethyl)aniline, its application will become more common.

Reference:
Patent; Hatton; Leslie R.; Buntain; Ian G.; Hawkins; David W.; Parnell; Edgar W.; Pearson; Christopher J.; Roberts; David A.; US5232940; (1993); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 201849-21-0,Some common heterocyclic compound, 201849-21-0, name is 4-Bromo-2-chloro-1-isopropoxybenzene, molecular formula is C9H10BrClO, 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.

A mixture of Compound 27B (1.35 g, 5.4mmol), Pd(dppf)C12 (0.35 g, 0.43 mmol), 4,4,4,4,5,5,5?, 5?-octamethyl-2,2?-bi( 1,3 ,2-dioxaborolane) (2.09 g, 8.22 mmol), and potassium acetate (1.62 g, 16.5 mmol) in 1,4-dioxane (50 ml) was heated at 80C for 16 hours. The mixture was diluted with water (200 mL) and extracted with ethyl acetate (200 mL x 2). The combined extracts were washed with water (200 mL) and brine (200 mL), dried over anhydrous sodium sulfate, filtered, and concentrated. The residue was purified with flash column chromatography on silica gel (ethyl acetate in petroleum ether, from 0% to 10% v/v) to furnish Compound 27C. LC-MS (ESI) m/z: non-ionizable compound under routine conditions used.

The synthetic route of 201849-21-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHAO, Qi; (737 pag.)WO2019/133770; (2019); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1996-30-1, 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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To an oven-dried 25 mL Schlenk tube containing a stirring bar was added 4.5 mg Pd(OAc)2 (0.02 mmol), 15.7mg nBuPAd2 (0.44 mmol), 2-bromofluorobenzene (0.50 mmol), salicylaldehyde (0.50 mmol), potassium carbonate (1.0 mmol). The Schlenk tube was vacuumed and then purged with argon before DMF (2.0 mL) was injected using a syringe. Afterwards the Schlenk tube in the ice bath was degassed by evacuation and back fillingwith argon three times. The reaction mixture was then stirred for 12 h at 120 C. After the reaction was complete,the reaction mixture was diluted with water (5 mL), extracted with ethyl acetate (3 x 10 mL) and dried withanhydrous Na2SO4. After filtration and addition of silica gel into the solution, the organic solvent was reduced evaporated. The crude product was purified by column chromatography using ethyl acetate/n-pentane.

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, 3-Bromo-4-fluorochlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Shen, Chaoren; Wu, Xiao-Feng; Synlett; vol. 27; 8; (2016); p. 1269 – 1273;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, This compound has unique chemical properties. The synthetic route is as follows., category: chlorides-buliding-blocks

A mixture of 5-chloro-1/-/-benzotriazole (8 g), chloroacetone (6.5 ml_), potassium carbonate (9.5 g) and potassium iodide (0.5 g) was stirred in acetone (90 ml.) at room temperature for 48 hours. The reaction mixture was filtered and the filtrate concentrated under reduced pressure to give a residue that was purified by chromatography (SiO2, heptane/EA) to afford 1-(5-chloro-2H-benzotriazol-2-yl)-propan-2-one as clear oil [1.8 g, 16%, Rf =0.6 (1 :1 EA/heptane)]. The two other regioisomers were also isolated, 1-(6- chloro-1 H-benzotriazol-1-yl)-propan-2-one [3.8 g, 35%, Rf =0.45 (1 :1 EA/heptane)] and 1- (5-chloro-1H-benzotriazol-1-yl)-propan-2-one [3.2 g, 29%, Rf =0.35 (1 :1 EA/heptane)].

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 94-97-3.

Reference:
Patent; MERIAL LIMITED; AVENTIS AGRICULTURE; WO2008/144275; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics