Category: chlorides-buliding-blocks

Synthetic Route of 139512-70-2, These common heterocyclic compound, 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine, 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 mixture of compound 11 (0.46 mmol) and appropriate o-phenylenediamines (0.46 mmol) in ethanol was added a solution of Na2S2O5 (770 mg, 4 mmol) in H2O (1.6 mL). The resulting mixture was stirred at reflux for 4 h. after completion of reaction; the solution was evaporated under reduced pressure to remove ethanol, and partitioned between EtOAc and water. The organic layer was dried over Na2SO4, and concentrated in vacuo. The crude product was purified by column chromatography using EtOAc/hexane as eluant to afford pure compounds 12(a-l) in good yields.

The synthetic route of 139512-70-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kamal, Ahmed; Srinivasa Reddy; Polepalli, Sowjanya; Shalini, Nekkanti; Reddy, V. Ganga; Subba Rao; Jain, Nishant; Shankaraiah, Nagula; Bioorganic and Medicinal Chemistry; vol. 22; 19; (2014); p. 5466 – 5475;,
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Application of 108-37-2,Some common heterocyclic compound, 108-37-2, name is 1-Bromo-3-chlorobenzene, molecular formula is C6H4BrCl, 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 solution of i-butyl piperazine-l-carboxylate (1.96 g, 10.54 mmol, 2.00 equiv), 1- bromo-3-chlorobenzene (1 g, 5.26 mmol, 1.00 equiv), BINAP (330 mg, 0.53 mmol, 0.10 equiv), Pd2(dba)3 (243.8 mg, 0.27 mmol, 0.05 equiv), NaOi-Bu (1.59 g, 16.56 mmol, 3.00 equiv), and toluene (17 mL) was placed in a 100-mL round bottom flask, stirred overnight at 100C in an oil bath, and concentrated under vacuum. Purification via silica gel column (PE/EA (50:1)) yielded 1.3 g (83%) of i-butyl 4- (3-chlorophenyl)piperazine-l-carboxylate as a yellow solid. LC-MS (ES, m/z): 297 [M+H]+

The synthetic route of 108-37-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOENERGENIX; MCCALL, John, M.; MCKEARN, John; ROMERO, Donnal, L.; CLAIR, Michael; WO2011/28947; (2011); A2;,
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. 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C13H11ClFNO

(I) Preparation of the compounds Example 1: Preparation of N-{4-[3-chloro-4-(3-fluoro-benzyloxy)phenylamino] quinazolin-6-yl}-acrylamide 3tep A: preparation of 4-[3-chloro-4-(3-fluoro-benzyloxy)phenylamino]-6-nitro-quinazoline 1.20 g (5.7 mmol) of 4-chloro-6-nitro-quinazoline (prepared by referring to WO 2007/082434) and 1.37 g (5.6 mmol) of 4-(3-fluoro-benzyloxy)-3-chloro-aniline (prepared by referring to WO 2007/082434) were dissolved in 80mL of isopropanol and refluxed for 3 hours. A large amount of yellow solid was precipitated from the system, and was filtered. The filter cake was washed with a saturated sodium bicarbonate aqueous solution till pH=8 and dried under vacuum to give 1.62g ( 3.75 mmol ) of yellow solid, which was identified as 4-[3-chloro-4-(3-fluoro-benzyloxy) phenylamino]-6-nitro-quinazoline with a yield of 67%. 1H-NMR (400MHz, CDCl3): delta 11.30(1H, br), 9.54-9.48(1H, m), 8.45-8.41(1H, m), 8.31-8.25(1H, m), 7.98-7.89(1H, m), 7.50-7.47(1H, m), 7.35-7.26 (1H, m), 7.05-6.96(1H, m), 6.90-6.80(2H, m), 7.74-7.60(2H, m), 4.84(2H, s).

The synthetic route of 202197-26-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Allist Pharmaceuticals, Inc.; EP2292234; (2011); 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. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 2,4-Difluorobenzene-1-sulfonyl chloride

Intermediate 36: 2,4-Difluoro-N-(2-hydroxyethyl)-N-methyl-benzenesulfonamide 2,4-Difluorobenzenesulfonyl chloride (CAS no. 13918-92-8) (4.0 g, 19 mmol) in DCM (10 mL) was added slowly to a solution of 2-(methylamino)ethanol (1.66 mL, 20.7 mmol) in DCM (200 mL) and 10% sodium hydroxide solution (200 mL) at 0 C. The reaction was allowed to warm to room temperature and stirred for 20 hours. The DCM layer was separated and the aqueous re-extracted into DCM (2*50 mL). The combined organic extracts were washed with brine (200 mL), dried (MgSO4), filtered and evaporated under reduced pressure to afford the product (4.7 g, 98%). 1H NMR 6 (400 MHz, CDCl3): 1.98 (t, 1H), 2.94 (s, 3H), 3.32 (t, 2H), 3.79 (q, 2H), 6.94-7.03 (m, 2H), 7.89-7.95 (m, 1H).

The synthetic route of 13918-92-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AstraZeneca AB; US2008/171734; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 445-13-6, name is 3-Chloro-4-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., Recommanded Product: 3-Chloro-4-(trifluoromethyl)aniline

iV-tS-CIiloro^-CtrifluoromethylJphenyy^-fCl-methylpiperidin-S- yl)methyl]pipera-ne-l-carboxaniotaide; To a solution of di-tert-butyl dicarbonate (114.6 mg) in chloroform (2 ml) was added 4-dimethylaminopyridine (6 mg). A solution of 4-amino-2-chlorobenzotrifluoride(98.1 mg) in chloroform (2 ml) was added and the reaction mixture stirred for 20 minutes at room temperature. A solution of l-[(l-methylpiperidm-3-yl)methyl]piperazine (98.5 mg) in chloroform (2 ml) was added and the resulting solution was stirred at reflux for 18 hours. The reaction mixture was purified by column chromatography on silica gel (20 g) using a gradient of 100% dichloromethane through to 20% methanolic ammonia in dichloromethane to give the title compound (14 mg).

The synthetic route of 445-13-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/67401; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2533-69-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2533-69-9 name is Methyl 2,2,2-trichloroacetimidate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

(a) First step: preparation of 2-trichloromethyl-1H-benzimidazole: Methyl trichloroacetimidate (12.8 ml, 0.103 mol) was added dropwise over 30 minutes to 1,2-phenylenediamine (10.8 g, 0.1 mol) dissolved in 250 ml of acetic acid at 150 C. and with stirring. The mixture was maintained under stirring for 5 hours at room temperature. The reaction mixture and poured into water. The precipitate formed was filtered off, washed with water and dried. 23.1 g (yield=98%) of an off-white powder of 2-trichloromethyl- 1H-benzimidazole were obtained.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 2,2,2-trichloroacetimidate, and friends who are interested can also refer to it.

Reference:
Patent; Societe L’Oreal S.A.; US6221343; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 39226-95-4, name is 2,3-Dichlorobenzylamine, 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 39226-95-4, Recommanded Product: 2,3-Dichlorobenzylamine

2-Bromo-4-(2,3-dichlorobenzylamino)-5-nitropyridine (2); [0087] To a solution of 2,4-dibromo-5-nitropyridine (1) (0.5 g, 1.77 mmol) in THF (10 mL) at 0 C was added a mixture of 2,3-dichlorobenzylamine (0.32 g, 1.82 mmol), diisopropylethylamine (0.62 mL, 3.56 mmol), and THF (10 mL) dropwise with stirring under argon. After addition, the resulting mixture was stirred at room temperature for 5 h when TLC analysis (EtOAc-hexanes, 1:4) showed that the reaction was complete. The mixture was then poured into cold water (60 mL) and extracted with DCM (2 x 60 mL). The combined organic layers were washed with brine, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by column chromatography (EtOAc-hexanes, 1 :6) to give 2 as a yellow solid (605 mg, 91%). LC-MS: Rt 7.72 min, m/e 378.0; 1H NMR (CDCl3) delta 9.00 (s, 1 H), 8.57 (s, broad, 1 H, NH), 7.48 (d, 1 H), 7.23 (d, 1 H), 7.18 (m, 1 H), 6.82 (s, 1 H), 4.61 (d, 2 H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,3-Dichlorobenzylamine, and friends who are interested can also refer to it.

Reference:
Patent; PHARMACOPEIA, INC.; WO2009/62059; (2009); A2;,
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. 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8H9ClO4S

General procedure: To a solution of hydrogen chloride gas in dry ethyl acetate (1.5 M,3.0 mL) was added intermediate IM 3 (0.3 g, 0.6 mmol). The reactionmixture was stirred for 4 h at room temperature. The solvent was removedunder reduced pressure to give solid deprotected product.Various substituted-phenyl sulfonyl chlorides were added dropwise in a mixture of deprotected product and triethylamine (0.5 mL) in anhydrousCH2Cl2 (10 mL). After stirring at room temperature overnight, thereaction mixture was concentrated using a rotary evaporator. The crudeproduct was purified by chromatography on silica gel utilized a mixtureof chloroform and acetone (35:1, v/v) as eluent to furnish the desiredproduct.

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 63624-28-2.

Reference:
Article; Yuan, Lei; Liu, Jun; He, Wenhui; Bao, Youmei; Sheng, Lei; Zou, Chunyang; Hu, Baichun; Ge, Wentao; Liu, Yang; Wang, Jian; Lin, Bin; Li, Yanchun; Ma, Enlong; Bioorganic Chemistry; vol. 84; (2019); p. 239 – 253;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 102-49-8, name is 3,4-Dichlorobenzylamine, A new synthetic method of this compound is introduced below., Computed Properties of C7H7Cl2N

General procedure: Compound 12a, 12b or 12c (0.55 mmol), the appropriate amine(1.1 mmol) and 1,2-dimethoxyethane (1 mL) were heated in amicrowave reactor (150 Watt, Power Max On, 90 C, 10 bar) for1 h. The solvent was removed under reduced pressure and the residuewas purified by column chromatography (silica gel, ethylacetate).

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; Koch, Pierre; Akkari, Rhalid; Brunschweiger, Andreas; Borrmann, Thomas; Schlenk, Miriam; Ku?ppers, Petra; Ko?se, Meryem; Radjainia, Hamid; Hockemeyer, Jo?rg; Drabczyn?ska, Anna; Kiec?-Kononowicz, Katarzyna; Mu?ller, Christa E.; Bioorganic and Medicinal Chemistry; vol. 21; 23; (2013); p. 7435 – 7452;,
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. 367-22-6, name is 4-Chloro-3-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H5ClFN

N-(4-Chloro-3-fluorophenyl)-4-nitropyridin-3-amine NaH (422 mg, 60% dispersion in mineral oil, 10.6 mmol) was suspended in THF (20 mL) and 4-chloro-3-fluoroaniline (1.54 g, 10.6 mmol) and 3-fluoro-4-nitropyridine (500 mg, 3.52 mmol) were added. The reaction mixture was stirred for 18 h, quenched with sat aq NH4Cl (2 mL), and concentrated in vacuo. The residue was partitioned between water (50 mL) and DCM (50 mL) and the organic fraction was dried (MgSO4) and concentrated in vacuo. The residue was purified by column chromatography to give the title compound (207 mg, 22.0%) as an orange solid. LCMS (ES+): 268.0 [MH]+.

According to the analysis of related databases, 367-22-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Proximagen Limited; Espensen, Max; Patient, Lee; Evans, David; Savory, Edward; Simpson, Iain; US2014/275040; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics