Month: June 2021

Application of 918538-05-3, 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. 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

j00535j Compound rac**A2 (50 mg, 0.3 mmol) and 2,4-dichloropyrrolo[2,1-JI[1,2,4jtriazine (52 mg, 0.3 mmol) were dissolved in 2-propanol (1 mL). After stirring at room temperature for 3 hours, N,N-diisopropylethylamine (80 .iL, 0.5 mmol) was added, and the reaction mixture was stirred for 16 hours, concentrated onto silica and purified by column chromatography [chloroform: 7M NH3 in methanol = 1:0 to 9:11 to afford compound rac-6-int (59 mg, 64% yield). LCMS (1): tR=2.498 mi, (ES) m/z (M+H) = 333.0.

The synthetic route of 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FORUM PHARMACEUTICALS, INC.; ACHARYA, Raksha; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; COOK, Andrew, Simon; HARRISON, Bryce, Alden; McRINER, Andrew, J.; (267 pag.)WO2017/69980; (2017); A1;,
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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. 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, This compound has unique chemical properties. The synthetic route is as follows., name: 5-(Chloromethyl)benzo[d][1,3]dioxole

Preparation of 1, 3-benzodioxol-5-ylmethyl isopropyl sulfone 7.8 g of 5-(chloromethyl)-1, 3-benzodioxol was dissolved in 20 ml of anhydrous tetrahydrofuran and 20 ml of diethyl ether and then added to magnesium at 0C, and reacted for 10 minutes. The reactant was heated to 50C and reacted for 1 hour. The reaction mixture was cooled to 0C and then slowly added to a flask containing [1, 3-bis (diphenylphosphino) propane] nickel (II) dichloride as a catalyst. After the addition of 3. 9 ml isopropane sulfonyl chloride, the mixture was reacted for 30 minutes and the reactant was heated to 50C and reacted for 1 hour. Then, its pH was adjusted to 7 with dilute hydrochloric acid. The resulting mixture was extracted with diethyl ether and distilled water, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was fractionated by column chromatography using ethyl acetate: n-hexane (1: 3), to give 0.6 g of the title compound of the following formula ld (Rf : 0.35, Yield: 5%). [Chemical Formula 1d] The compound was dissolved in CDC13 and TMS and then characterized by IH NMR spectroscopy. The result is as follows ; ‘H NMR 8 : 1.60-1. 62 (d, 6H, J=6.7Hz), 2.79 (s, 2H), 3.75-3. 78 (m, 1H), 5.91 (s, 2H), 6.66 (m, 3H)

According to the analysis of related databases, 20850-43-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HAN, Sang Min; LEE, Myung Hee; CHOI, Won Chul; WO2005/70915; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 328-84-7, These common heterocyclic compound, 328-84-7, name is 3,4-Dichlorobenzotrifluoride, 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.

Example 1 2,3-dichloro-6-trifluoromethylbenzoic acid (Compound No. 11) STR17 83.4 g of 3,4-dichlorobenzotrifluoride was dissolved in 800 ml of dried tetrahydrofuran, and 250 ml of hexane solution of n-butyl lithium(1.6 mol/1) was added to the solution dropwise over 15 minutes at -78 C. under nitrogen atmosphere. Following to stirring the solution for 2 hours at -78 C., 50 g of dry ice was then gradually added to the solution at the same temperature. After elevating the temperature of the solution up to room temperature, 250 ml of cold water was added to the solution to separate the resulting solution, and the aqueous layer obtained was adjusted to an acidic condition of a pH value of 1 with concentrated hydrochloric acid while cooling. Then, the aqueous layer was extracted with ether, and the extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled out under reduced pressure, and the oily residue obtained was crystalized with n-hexane, washed, filtered, and dried to obtain 89 g of the title compound(mp. 88-89 C.).

Statistics shows that 3,4-Dichlorobenzotrifluoride is playing an increasingly important role. we look forward to future research findings about 328-84-7.

Reference:
Patent; Nippon Soda Co., Ltd.; US6054605; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 102-49-8, 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. 102-49-8, name is 3,4-Dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 2,2,2-Trichloro-1-(4,5-dibromo-1H-pyrrol-2-yl)ethanone (3) (0.200 g, 0.54 mmol), and phenylmethanamine (0.058 g, 0.06 mL, 0.54 mmol) were dissolved in acetonitrile (10.0 mL). Triethylamine (5 equiv, 0.38 mL) was added to the solution, and the reaction mixture stirred at 60 °C for 24 h. Solvent was removed from the reaction by rotary evaporation. The resulting yellow oil was purified using column chromatography from 2percent MeOH/CH2Cl2 to afford N-benzyl-4,5-dibromo-1H-pyrrole-2-carboxamide (0.0978 g, 51percent) as a brown solid, decomp. 125 °C.

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

Reference:
Article; Dyson, Lauren; Wright, Anthony D.; Young, Kelly A.; Sakoff, Jennette A.; McCluskey, Adam; Bioorganic and Medicinal Chemistry; vol. 22; 5; (2014); p. 1690 – 1699;,
Chloride – Wikipedia,
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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. 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, A new synthetic method of this compound is introduced below., Safety of 3-Chloropropan-1-amine hydrochloride

General procedure: Toa suspension of lawsone (0.87 g, 5.0 mmol) in ethanol(10 mL) were added sequentially: i) the corresponding amine (5.5 mmol) – andtriethylamine (5.0 mmol, 0.7 mL) in the case of 3-(chloropropyl)aminehydrochloride – and ii) the respective aldehyde (6.0 mmol). The reactionmixture was stirred at RT, in the dark for 12h, after which time the orangeprecipitate was filtered, washed with ethanol, diethyl ether and dried undervacuum.Forthe syntheses of 6a, 6b, 6e, 6f, 6g and 6h, which are more soluble than the other products, the reactionswere carried out in the same amount of ethanol, but using 10.0 mmol of lawsone,10.0 mmol of heptylamine and 12.0 mmol of aldehydes.Compounds4a, 5a, 8a, 4b, 5b, 4c, 5c, 4d, 5d, 6d, 7d, 8d, 9e, 5g, 4h and 5h were synthesized as describedpreviously.3-5

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; da Silva, Gustavo B.; Neves, Amanda P.; Vargas, Maria D.; Marinho-Filho, Jose D.B.; Costa-Lotufo, Leticia V.; Bioorganic and Medicinal Chemistry Letters; vol. 26; 15; (2016); p. 3537 – 3542;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 1005-56-7,Some common heterocyclic compound, 1005-56-7, name is O-Phenyl carbonochloridothioate, molecular formula is C7H5ClOS, 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.

In a 30 ml eggplant type flask,Methyl alpha-L-rhamnopyranoside178.2 mg (1.0 mmol),Dioctyldichlorotin41.6 mg (0.10 mmol),Tetrabutylammonium iodide36.9 mg (0.10 mmol),Tetrahydrofuran10 ml was added,Followed by stirring.thisTo the mixed solution, phenyl chlorothionoformate0.175 ml (1.3 mmol) was added,Then,1,2,2,6,6-pentamethylpiperidine0.271 ml (1.5 mmol) was added,The reaction was carried out at 20 C. for 6 hours.After completion of the reaction,To the reaction solution was added saturated ammonium chloride aqueous solution (20 ml)The extraction operation was carried out three times with 20 ml of ethyl acetate.The organic phase (ethyl acetate phase) was washed with 20 ml of water,After washing with 20 ml of an aqueous sodium chloride solution,It was dried over anhydrous magnesium sulfate,After filtration,The solvent (ethyl acetate) was distilled off under reduced pressure.The residuePurification by silica gel chromatography(Developing solvent n – hexane: ethyl acetate = 5: 1), 299.2 mg (yield 95%) of methyl 3 – O – phenoxythiocarbonyl -alpha- L – rhamnopyranoside was obtained. The hydroxyl groups other than the 3-position are monophenoxythiocarbonylatedThe selectivity of methyl 3-O-phenoxythiocarbonyl-alpha-L-rhamnopyranoside was 100% because alpha-L-rhamnopyranoside was not obtained.

The synthetic route of 1005-56-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NAGASAKI UNIVERSITY; TOKUYAMA CORPORATION; ONOMURA, OSAMU; MURAMATSU, WATARU; IWASAKI, FUMIAKI; (32 pag.)JP5669643; (2015); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 32768-54-0, These common heterocyclic compound, 32768-54-0, name is 2,3-Dichlorotoluene, 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: In a 1L reactor,add 61.5 g of 2,3-dichlorotoluene, 3.075 g of azobisisobutyronitrile (5%), 215.25 g of 2-dichloroethane, heat the mixture at 75 C and add 44 g of bromine drop wise,reflux reaction till red bromine fades , Intermittent drip and 136.2g27.5% hydrogen peroxide continues to react till red bromine no longer generates. Add a 49.2g30% aqueous solution of sodium carbonate to the reaction solution, reflux reaction for 8 h ,at the same time recover1,2-dichloroethane.

Statistics shows that 2,3-Dichlorotoluene is playing an increasingly important role. we look forward to future research findings about 32768-54-0.

Reference:
Patent; Lianyungang Industry Investment Group Co., Ltd.; Jiang Honglai; Jiang Xiao; Han Yong; Zang Han; Zhu Chengjie; Shen Weiwei; (5 pag.)CN107032968; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1127-85-1, 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. 1127-85-1, name is 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of 2,4-dichloropyrrolo[1,2-f][1,2,4]triazine (4a) (0.5 g, 2.7 mmol) in 2-Propanol (6 mL) was added (S)-pyrrolidin-2-ylmethanol (0.39 mL, 4.0 mmol), DIPEA (1.39 mL, 8.0 mmol) and heated at 90 C for 1 hr. The reaction was cooled to room temperature and solid obtained was collected by filtration to afford (S)-(l-(2-chloropyrrolo[2,l-f][l,2,4]triazin-4- yl)pyrrolidin-2-yl)methanol (96a) (0.49 g, 73 % yield) as a white solid; NMR (300 MHz, DMSO-i/e): delta 7.70 (dd, J= 2.6, 1.4 Hz, 1H), 6.97 (dd, J= 4.7, 1.6 Hz, 1H), 6.80 – 6.57 (m, 1H), 5.15 (t, J = 5.7 Hz, 1H, D2O exchangeable), 4.87 (t, J= 5.7 Hz, 1H), 4.44 (d, J= 17.8 Hz, 1H), 4.05 – 3.82 (m, 1H), 3.72 – 3.39 (m, 2H), 2.22 – 1.84 (m, 4H). MS (ES+): 253.3, 255.3 (M+2); MS (ES-): 287.2, 289.2 (M+Cl).

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, 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BIOCRYST PHARMACEUTICALS, INC.; KOTIAN, Pravin, L.; BABU, Yarlagadda, S.; KUMAR, V., Satish; ZHANG, Weihe; LU, Peng-Cheng; RAMAN, Krishnan; (747 pag.)WO2018/232094; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. SDS of cas: 19752-55-7

After mixing compound 3-3 (10 g, 0.02 mol), 1-bromo-3,5-dichlorobenzene (7.2 g, 0.03 mol), tetrakis(triphenylphosphine)palladium(O) (0.92 mg, 0.79 mmol), sodium carbonate (5.6 g, 0.05 mol), toluene 130 mL, ethanol 33 mL, and distilled water 33 mL in a flask, the mixture was stirred at 120°C for 12 hours. After completing the reaction, the mixture was extracted with ethylacetate, and the obtained organic layer was dried with anhydrous magnesium sulfate and filtered. The solvent was then removed under reduced pressure, and the remaining substance was subjected to column chromatography to separate compound 3-4 (4.4 g, 35percent).

The synthetic route of 19752-55-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ROHM AND HAAS ELECTRONIC MATERIALS KOREA LTD.; AHN, Hee-Choon; YANG, Soo-Jin; MOON, Doo-Hyeon; JUN, Ji-Song; LEE, Tae-Jin; LEE, Kyung-Joo; KWON, Hyuck-Joo; KIM, Bong-Ok; WO2014/98518; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 2770-11-8, name is 2-(4-Chlorophenoxy)aniline, molecular formula is C12H10ClNO, 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. Quality Control of 2-(4-Chlorophenoxy)aniline

A stirred solution of Boc-glycine (1.50 mmol), PyBOP (1.60 mmol) and DIPEA (3.50 mmol) in dichloromethane (10 mL) was cooled to 0 C with an ice bath. To this solution 2-(4-chlorophenoxy)aniline (1.50 mmol), dissolved in a minimum amount of dichloromethane, was added dropwise. The reaction mixture was allowed to warm to room temperature and was then stirred for 24 h. Thereafter, an aqueous work-up was performed similar to that of compounds 1-8. The resulting oil was further purified by column chromatography over silica gel(dichloromethane/methanol 200:1) to give a slightly orange solid (358 mg, 0.95 mmol, 63%); m.p.: 50-51 C; IR (KBr): [cm-1] nu = 3409 (m, N-H), 3342 (s, N-H), 1691 (br, s, C=O); 1H-NMR: (600 MHz, DMSO-d6): delta [ppm] = 1.34 (s, 9H, CH3), 3.71 (d, J = 6.1 Hz, 2H, CH2), 6.87-7.06 (m, 3H, arom. H), 7.05-7.30 (m, 3H, arom. H), 7.35-7.53 (m, 2H, arom. H), 8.12 (d, J = 7.7 Hz, 1H, NH), 9.33 (s, 1H, NH); 13C-NMR (151 MHz, DMSO-d6) delta [ppm] = 28.00 (3C, CH3), 43.92 (CH2), 118.82, 119.90 (2C), 122.35, 124.15, 124.63, 129.70 (2C) (CH), 78.17, 127.17, 129.64, 146.09, 155.47, 155.86, 168.51 (C); EI-MS: m/z (%): 376.1 [M]+ (11), 219.1 [M – 157]+ (100); HREI-MS: calcd. for C19H21ClN2O4 376.11844, found 376.11803; HPLC: 96.3% at 254 nm, 96.3% at 280 nm; tR = 4.84 min, tM(DMSO) = 1.06 min(ACN/H2O = 60:40), lambdamax [nm] = 230; HPLC-gradient: 95.8%, tR = 12.80 min, tM(DMSO) = 1.28 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2770-11-8, its application will become more common.

Reference:
Article; Weidner, Thomas; Nasereddin, Abed; Preu, Lutz; Gruenefeld, Johann; Dzikowski, Ron; Kunick, Conrad; Molecules; vol. 21; 2; (2016);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics