Category: 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. 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., Quality Control of 5-Chloro-1H-benzo[d][1,2,3]triazole

To a solution of 5-chloro-1H-benzotriazole (1 g) and sodium acetate (1g) in acetic acid was added bromine (2 g). After 10 days at room temperature, the mixture was treated with a saturated solution sodium thiosulfate, neutralized with a saturated solution of sodium bicarbonate and extracted with ethyl acetate. The organic phase was washed with brine, dried over anhydrous sodium sulfate, filtered and the filtrate concentrated under reduced pressure to afford a residue that was purified by semi- preparative liquid chromatography to afford 4-bromo-5-chloro-1 /-/-benzotriazole as an off-white solid (213 mg, 14%). MS (ES): M/Z [M+H]=232. 1H NMR: (400 MHz, DMSO-dbeta): 7.58 (d, J =8.7 Hz, 2H) and 7.91 (d, J =8.7 Hz, 1H).

According to the analysis of related databases, 94-97-3, the application of this compound in the production field has become more and more popular.

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

Adding a certain compound to certain chemical reactions, such as: 104-52-9, name is 3-Phenylpropyl Chloride, 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 104-52-9, Recommanded Product: 3-Phenylpropyl Chloride

EXAMPLE 2 Preparation of 3-phenoxy-3-phenylpropylamine A reaction mixture consisting of 1000 g. of 3-chloropropylbenzene, 1500 g. of N-bromosuccinimide, 5 g. of benzoyl peroxide and 6 l. of carbon tetrachloride were placed in a 12 l. 3-neck, round-bottom flask equipped with stirrer and condenser. The reaction mixture was stirred and heated until an exothermic reaction began. The heat source was then removed, after the exothermic reaction had subsided, the reaction mixture was refluxed until the reaction was completed as noted by the disappearance of the N-bromosuccinimide. The reaction mixture was then cooled and crystalline succinimide collected by filtration. The succinimide filter cake was washed with carbon tetrachloride. The combined filtrate and wash was concentrated in vacuo. The residue comprising 3-chloro-1-bromopropylbenzene obtained in the above reaction, was shown by a NMR to be the desired material and was used without further purification.

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-Phenylpropyl Chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Eli Lilly and Company; US4313896; (1982); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 104-52-9, name is 3-Phenylpropyl Chloride, 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 104-52-9, Computed Properties of C9H11Cl

2.1 g of compound 1 was dissolved into 15mL of DMF, add 1.39 g of potassium carbonate, stir at 50 C with heating, add the drops of 3-phenylpropyl chloride (1.55g), heat to reflux, and react for 2h, and then cool at 60 C, added the drops of Diphenyl methylamine (1.83g), heat again to reflux, carry on reaction for 1.5h, after the reaction, filter, filter cake washed with a small amount of DMF, the filtrate is distilled off under reduced pressure, add 15g of ice water, stir, and filter and obtained a crude product, adding the crude product to methanol and then, it is made into salt with concentrated hydrochloric acid, by filter obtained hydrochloride salt of compound I-3, hydrochloride added into 6mL of water, adjust adjusting the pH at 8 with ammonium hydroxide and obtain a large amount of white powder, filter, dry, i.e. obtained Compound I-3 (3.34g, yield is 70.3%).

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

Reference:
Patent; Suzhou Huazhen Pharmaceutical Technology Co., Ltd.; Ma Lihua; Su Longzhen; Shi Xiaohui; (8 pag.)CN108358855; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 60811-18-9, These common heterocyclic compound, 60811-18-9, name is 4-Bromo-1-chloro-2-fluorobenzene, 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.

1-Bromo-4-chloro-3-fluorobenzene (1 g, 4.8 mmol), bis(pinacolato)diboron (1.33 g, 5.3 mmol), potassium acetate (1.4 g, 14.3 mmol) and bis(triphenylphosphine)palladium dichloride (0.2 g, 0.29 mmol) were suspended in dioxane (20 ml). The yellow suspension was flushed with argon for 30 minutes and refluxed for 12 hours. The reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue was chromatographed over silica gel (hexane-ethyl acetate 99:1) to provide 2-(4-chloro-3-fluoro-phenyl)-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (0.7 g, 59%) as a colorless oil, MS: m/e=256.2 (M+).

Statistics shows that 4-Bromo-1-chloro-2-fluorobenzene is playing an increasingly important role. we look forward to future research findings about 60811-18-9.

Reference:
Patent; Buettelmann, Bernd; Neidhart, Marie-Paule Heitz; Jaeschke, Georg; Pinard, Emmanuel; US2003/229096; (2003); 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. 39065-95-7, name is 4-(Chlorodifluoromethoxy)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C7H6ClF2NO

[00542] (R)-6-(3-Hydroxypyrrolidin-l-yl)-5-(pyrimidin-5-yl)nicotinic acid (Stage 170.1, 57.3 mg, 0.2 mmol), HOBT (43.5, 0.284 mmol) and EDC (42.2 mg, 0.22 mmol) were dissolved in 0.3 M NMM in DMF (0.8 niL) at RT. 4-(Chlorodifluoromethoxy)aniline (36.8 mg, 0.19 mmol) was added and the RM was stirred for 5 h. The RM was then diluted with EtOAc and washed with 10% NaHCC>3. The organic layer was dried over Na2S04, filtered and evaporated to dryness under reduced pressure. The residue was purified by flash chromatography (RediSep Silica gel column, DCM / MeOH, from 2 to 5% MeOH) and treated with Si-Thiol (50 mg) in MeOH to afford the title compound. HPLC Chiral (CHIRALPAK AD-H, 250 x 4.6 mm, eluent : EtOH/MeOH (50:50), 0.5 mL/min, UV 210 nm) tR = 21.89 min, UPLC-MS (Condition 3) tR = 0.95 min, m/z = 462.2 / 464.2 [M+H]+; XH-NMR (400 MHz, DMSO-d6) delta ppm 1.67 – 1.78 (m, 1 H) 1.80 – 1.89 (m, 1 H) 2.87 (d, J = 11.34 Hz, 1 H) 3.21 (m, J = 11.10, 4.90 Hz, 2 H) 3.33 – 3.44 (m, 1 H) 4.12 – 4.24 (m, 1 H) 4.87 (d, J = 3.52 Hz, 1 H) 7.33 (d, J = 8.60 Hz, 2 H) 7.77 – 7.89 (m, 2 H) 8.08 (d, J = 2.35 Hz, 1 H) 8.78 (d, J = 2.35 Hz, 1 H) 8.88 (s, 2 H) 9.18 (s, 1 H) 10.17 (s, 1 H).

The synthetic route of 39065-95-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; FURET, Pascal; GROTZFELD, Robert Martin; JONES, Darryl Brynley; MANLEY, Paul; MARZINZIK, Andreas; PELLE, Xavier Francois Andre; SALEM, Bahaa; SCHOEPFER, Joseph; SPIESER, erich Alois; WO2013/171640; (2013); A1;,
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. 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Chloro-4-fluorobenzylamine

A mixture of intermediate 59 (200 mg, 0.54 mmol), 2-chloro-4-fluorobenzylamine (0.5 mL, 3.76 mmol) is heated at 100 C. (reaction block) for 2 days. The reaction mixture is cooled to RT. The corresponding N-Boc intermediate is not isolated. The reaction mixture is dissolved in EtOAc (10 mL) and hydrogen chloride is bubbled into the solution for 1 min, and the solution is stirred at RT overnight. The reaction mixture is neutralized, the solvent is evaporated, and the residue is purified by chromatography on silica gel; gradient elution with heptane:EtOAc (70:30-50:50) gives 73 mg of the product 101. LC/MS: 1.78 min, m/z 380 (M++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 15205-11-5.

Reference:
Patent; Aventis Pharmaceuticals Inc.; US2005/26916; (2005); 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. 15205-15-9, name is 2-Chloro-6-fluorobenzylamine, A new synthetic method of this compound is introduced below., COA of Formula: C7H7ClFN

General procedure: 2-Amino-5-bromonicotinic acid (250 mg, 1.15 mmol) was dissolved in 4 ml of DMF. The solution was cooled in an ice bath. Then to the solution were successively added HATU (460 mg, 1.21 mmol), DIPEA (210.68 mul, 1.21 mmol), (2,3-difluorophenyl)methanamine (173 mg, 1.21 mmol). The resulting solution was stirred at room temperature for 2 h and then the saturated sodium bicarbonate solution was added. The mixture was extracted with ethyl acetate (EA). The combined organic layers were dried over anhydrous Na2SO4 and concentrated under vacuum. The crude product was used in the next step without purification.

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, Dengyou; Ai, Jing; Liang, Zhongjie; Li, Chunpu; Peng, Xia; Ji, Yinchun; Jiang, Hualiang; Geng, Meiyu; Luo, Cheng; Liu, Hong; Bioorganic and Medicinal Chemistry; vol. 20; 17; (2012); p. 5169 – 5180;,
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. 6781-98-2, name is 2-Chloro-1,3-dimethylbenzene, A new synthetic method of this compound is introduced below., Product Details of 6781-98-2

General procedure: A test tube was charged with aryl chlorides (0.5 mmol, 1 eq), arylboronic acid (0.75 mmol, 1.5 eq), K3PO4 (1 mmol, 2 eq), H2O (0.5 mL), isopropanol (0.5 mL) and catalyst (0.0005-0.001 mmol) and the mixture was then stirred at room temperature. After the reaction was finished, the mixture was extracted three times with CH2Cl2 (3 x 2mL), dried over Na2SO4, filtered, and the solvent was removed under vacuum. Further purification of the product was achieved by flash chromatography on a silica gel column.

The synthetic route of 6781-98-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Guiyan; Liu, Chengxin; Han, Fangwai; Wang, Zhongliang; Wang, Jianhui; Tetrahedron Letters; vol. 58; 8; (2017); p. 726 – 731;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 622-86-6, name is (2-Chloroethoxy)benzene, 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 622-86-6, name: (2-Chloroethoxy)benzene

A.27 Synthesis of [(PhOCH2CH2)2ImH]Cl (27) (2-chloroethoxy)benzene (5.02 g, 32.05 mmol) and l-(trimethylsilyl)imidazole (1.33 g, 9.48 mmol) and toluene (5 mL) were stirred at 1 10C for 7 days in complete darkness. The resultant biphasic mixture was cooled to room temperature and the top layer was discarded. The viscous bottom layer was dissolved in dichloromethane (1 mL) and pentane (50 mL) was added. The precipitated oil was washed with pentane (3×20 mL) and dried under high vacuum (3.27 g, quantitative). The product is an extremely viscous wax which solidifies completely over the course of several weeks. The following analytical data were obtained. *H NMR (CD2C12): delta 1 1.12 (s, 1H, NCHN), 7.57 (s, 2H, NCHCHN), 7.26 (t, 3JH-H= 7.7 Hz, 4H, m- CH), 6.97 (t, 4.8 Hz, 4H, 2xCH2), 4.39 (vt, 3JH-H= 4.8 Hz, 4H, 2xCH2). 13C NMR Patent; THE GOVERNING COUNCIL OF UNIVERSITY OF TORONTO; LANXESS Deutschland GmbH; MUELLER, Julia Maria; STEPHEN, Douglas; LUND, Clinton; SGRO, Michael; ONG, Christopher; CARIOU, Renan; WO2013/24119; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 38762-41-3, 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. 38762-41-3, name is 4-Bromo-2-chloroaniline, This compound has unique chemical properties. The synthetic route is as follows.

A. Tert-butyl N-(4-bromo-2-chlorophenyl)carbamate A solution of 4-bromo-2-chloroaniline (5.00 g, 0.0242 mol) in tetrahydrofuran (50 mL) was reacted with a 1.0 M solution of sodium bis(trimethylsilyl)amide in tetrahydrofuran (53.2 mL, 0.0532 mol). The mixture was stirred 15 minutes at ambient temperature. Di-tert-butyl dicarbonate (6.34 g, 0.0290 mol) was added and the solution was stirred for 2 hours. The solvent was removed in vacuo, and the crude material was purified by flash column chromatography on silica using heptane/ethyl acetate (4:1). The solvent was removed in vacuo to give tert-butyl N-(4-bromo-2-chlorophenyl)carbamate as a white solid (4.214 g, 0.0137 mol). 1H NMR (DMSO-d6, 400 MHz) delta 8.75 (s, 1H), 7.71 (d, 1H), 7.54 (d, 1H), 7.50 (dd, 1H), 1.46 (s, 9H);

The chemical industry reduces the impact on the environment during synthesis 4-Bromo-2-chloroaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Abbott Laboratories; US2002/156081; (2002); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics