Category: chlorides-buliding-blocks

Application of 174913-12-3, The chemical industry reduces the impact on the environment during synthesis 174913-12-3, name is 1-Bromo-3-chloro-5-methoxybenzene, I believe this compound will play a more active role in future production and life.

Step a: A solution of l-bromo-3-chloro-5-methoxybenzene (835 mg, 3.77 mmol), and l,3,5-trichloro-l,3,5-triazinane-2,4,6-trione (299 mg, 1.29 mmol) in DMF (18 mL) was stirred 16 h under N2 and 50 C. After cooling to RT, the reaction mixture was diluted with aqueous NH4C1 and extracted with Et20. The combined organic phases were dried over MgS04, filtered, concentrated, and the resulting residue was purified by silica chromatography (0 to 25% gradient of EtO Ac/heptane) to l-bromo-2,3-dichloro-5-methoxybenzene (720 mg, 2.81 mmol). 1H NMR (400 MHz, CHLOROFORM-^ delta ppm 7.14 (d, J=2.76 Hz, 1 H), 7.01 (d, J=3.01 Hz, 1 H), 3.81 (s, 3 H).

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, 1-Bromo-3-chloro-5-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NOVARTIS AG; CHEN, Zhuoliang; DORE, Michael; FORTANET, Jorge Garcia; KARKI, Rajesh; KATO, Mitsunori; LAMARCHE, Matthew J.; PEREZ, Lawrence Blas; WILLIAMS, Sarah; SENDZIK, Martin; WO2015/107494; (2015); 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. 2106-04-9, name is 3-Chloro-2-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3-Chloro-2-fluoroaniline

4. 0M HCI in Dioxane (4.0 ml) was added to a stirred suspension of 7- (benzyloxy)-4- chloro-6-methoxyquinazoline (CAS Registry NOL62364-72-9, prepared as described in W098/13354, Example 1) (60 g, 0.2 mol) and 3-CHLORO-2-FLUOROANILINE (31.96 g, 0.22 mol) in acetonitrile (1200 ml). The reaction mixture was heated at 80C for 1 hour then left to stand overnight. Acetonitrile (500 ml) was added and the resulting precipitate filtered, washed with acetonitrile (3 x 500 ml) and dried under vacuum to give 7- (BENZYLOXY)-N- (3-CHLORO-2- fluorophenyl) -6-methoxyquinazolin-4-amine hydrochloride as a beige solid (85.45 g, 96%);

According to the analysis of related databases, 2106-04-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2005/26150; (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. 870-24-6, name is 2-Chloroethanamine hydrochloride, A new synthetic method of this compound is introduced below., Formula: C2H7Cl2N

Step-I: 2-(2-Methyl-1H-pyrrol-1-yl)ethanamineSodium hydroxide anhydrous (9.87 g, 0.246 mol, 4.0 eq.) and TBAHS (0.838 g, 0.002 mol, 0.04 eq.) were added to a solution of 2-methyl-1 H-pyrrole (5.0 g, 0.061 mol, 1.0 eq.) in acetonitrile (180 ml) at 0 C and the mixture was stirred at RT for 1 h. 2-Chloroethylamine hydrochloride (8.59 g, 0.074 mol, 1.2 eq.) was added to the reaction mixture and it was then heated at reflux for 16 h. The reaction mixture was cooled to RT, filtered through celite and washed with 10% MeOH/DCM (200 ml). The filtrate was concentrated under reduced pressure to give the crude product which was used in the next step without further purification.Yield: 100 %, crude (7.6 g, 0.061 mol)

The synthetic route of 870-24-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GRUeNENTHAL GMBH; REICH, Melanie; SCHUNK, Stefan; OBERBOeRSCH, Stefan; JOSTOCK, Ruth; GERMANN, Tieno; ENGELS, Michael; WO2012/28331; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

771583-81-4, name is 4-Chloro-2-(trifluoromethyl)benzylamine, 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. name: 4-Chloro-2-(trifluoromethyl)benzylamine

4-chloro-2-trifluoromethylbenzylamine (100.0 mg, 0.5 mmol), 1-bromo-2-fluoroethane (78.7 mg, 0.6 mmol) and potassium carbonate (138.2 mg, 1.0 mmol) were dissolved in acetonitrile (5mL),The reaction was heated to 80 C for 4 hours. The reaction solution was cooled to room temperature. The reaction solution was concentrated. The concentrate was purified by preparative thin layer chromatography (eluent: petroleum ether: ethyl acetate = 4: 1 (v: v)) to obtain the title compound (40.0 mg, yield: 30%).

The synthetic route of 771583-81-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Kelun Botai Bio-pharmaceutical Co., Ltd.; Liu Chunchi; Liu Jinming; Cai Jiaqiang; Wang Lichun; Wang Jingyi; (25 pag.)CN110724076; (2020); A;,
Chloride – Wikipedia,
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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 1939-99-7 as follows. HPLC of Formula: C7H7ClO2S

A stirred solution of ethyl(3-amino-2-oxo-1,2-dihydropyridyl)acetate (40.0 g, 0.204 mole) and 2,4,6-collidine (54 ML, 0.408 mole) in tetrahydrofuran (200 ML) was cooled in an ice bath.. A solution of benzylsulfonyl chloride (38.9 g, 0.204 mmole) in tetrahydrofuran (200 ML) was added over a 50-minute period.. After addition was complete, the solution was stirred for 30 minutes at 0 C. The reaction mixture was diluted with ethyl acetate (1.2 L), washed with 1.0N HCl (until aqueous layer is PH 1), water (50 ML), saturated sodium bicarbonate (100 ML), and brine (2*50 ML).. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was removed.. The residue was recrystallized from chloroform. 39 g of the title compound was isolated.. To the mother liquor was added silica gel.. The solution was swirled, then filtered through a sintered glass funnel, washing with 50% ethyl acetate in dichloromethane.. The solvent was removed from the filtrate, and the residue was recrystallized from chloroform.. An additional 13 g of the title compound was isolated to afford a total of 52.00 g (75% yield) of the title compound as a tan solid. Rf=0.32 (silica gel, 20% ethyl acetate in dichloromethane); m.p. 48-49 C.

According to the analysis of related databases, 1939-99-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Corvas International, Inc.; US6342504; (2002); B1;,
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. 106-39-8, name is 1-Bromo-4-chlorobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C6H4BrCl

General procedure: To a mixture of aryl halide (0.3 mmol), NiCl2(H2O)1.5 [1] (0.0075 mmol, 2.5 mol percent), was charged dry THF (1 mL). The mixture was pumped and refilled with nitrogen for three times. The resulting mixture was stirred at -10 under nitrogen for 30 min. The reaction mixture was quenched through the addition of ice MeOH, then poured into a separatory funnel containing saturated aqueous NH4Cl (ca. 5 mL) and extracted with EtOAc (3 x 5 mL). The combined organic layers were washed with brine and dried over Na2SO4. The crude product was purified by column chromatography. Extent of isomerization can be easily determined via 1H NMR spectroscopy by comparison of the intergral of the singlet from the t-butyl group (1.3-1.4 ppm, 9H) to the integral of the doublet from the benzylic S3 protons of the i-butyl group (2.4-2.5 ppm, 2H). The doublet from the methyls of the i-butyl group could additionally be used (ca. 0.8 ppm, 6H).

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; Wu, Zhenghan; Si, Tengda; Xu, Guangqing; Xu, Bin; Tang, Wenjun; Chinese Chemical Letters; vol. 30; 3; (2019); p. 597 – 600;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 60811-18-9,Some common heterocyclic compound, 60811-18-9, name is 4-Bromo-1-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.

a. 4-chloro-3-fluorobenzoylpropionic acid To a solution of succinic anhydride (6.0 g) in tetrahydrofuran (60 ml) was added dropwise the Grignard prepared from 1.5 g (0.062 mole) of magnesium turnings and 10.5 g (0.05 mole) of 1-bromo-4-chloro-3-fluorobenzene using the procedure of part a. When the addition was completed, the resulting suspension was stirred for 2 hours at 45 C. after which water (100 ml) was added slowly and the resulting mixture was acidified with concentrated hydrochloric acid to pH=1. The ether layer was separated and extracted with 5% aqueous sodium hydroxide (3*100 ml). The combined aqueous solutions were washed with ether (1*100 ml). The combined basic aqueous layers were acidified with concentrated hydrochloric acid to pH 1 and extracted with ethyl acetate (3*150 ml). The combined organic extracts were washed with water (1*150 ml) and brine (1*150 ml), dried over anhydrous magnesium sulfate and evaporated in vacuo to give 7.1 g (62%) of the product as a yellow orange solid. The resulting acid was converted to the desired product using the procedure of Example 11d-e. Compound 83 was prepared following essentially the same procedure.

The synthetic route of 60811-18-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rohm and Haas Company; US5552409; (1996); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 29671-92-9, name is Carbamimidic chloride hydrochloride, 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 29671-92-9, COA of Formula: CH4Cl2N2

(1) Add methyl 3-amino-5-bromopyrimidinecarboxylate (6.2 g, 27 mmol) to a 250 mL sealed tube.Chloroformamidine hydrochloride (3.4 g, 30 mmol) and dimethyl sulfone (50.8 g, 20 mmol) were heated to 140oC and stirred for 6 hours. After cooling to room temperature, 50 mL of water was added to the reaction solution, followed by ultrasonication for 30 minutes. The residue was filtered. Water, acetone washing, vacuum drying to obtain a tan solid 1 (yield = 65%),

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, Carbamimidic chloride hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tsinghua University; Liao Xuebin; He Lei; Wang Zhisong; Gao Yan; (59 pag.)CN108069963; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 93765-83-4, 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. 93765-83-4, name is 1-Bromo-5-chloro-2-fluoro-4-methylbenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 12To a solution of 1-bromo-5-chloro-2-fluoro-4-methylbenzene (Comm, 10 g, 44.7 mmol) in methanol (200 ml_) was added 1 ,1′-binaphthalene-2,2′-diylbis(diphenylphosphine) – dichloropalladium (1:1) (358 mg, 0.447 mmol) and N,N-diethylethanamine (8.11 ml_, 58.2 mmol). The resulting mixture was placed in a bomb and pressurized with carbon monoxide to 80 psi and heated at 80C for 18 hours. The reaction mixture was then concentrated in vacuo to yield a semi-solid, which was dissolved in EtOAc (300 ml_) and washed with water (200 mL). The organic layer was separated, dried over magnesium sulphate, filtered and concentrated in vacuo to yield an orange oil, which solidified on standing (9.87 g). The solid was purified by silica gel chromatography eluting with 0 to 20% EtOAc in heptane to afford the title compound as a crystalline white solid (8.47 g, 93%).1H NMR (400 MHz, CDCI3): delta 2.40 (s, 3H), 3.92 (s, 3H), 7.03 (d, 1 H), 7.91 (d, 1 H) LCMS Rt = 1 .64 minutes Molecular ion not observed

The synthetic route of 1-Bromo-5-chloro-2-fluoro-4-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER LIMITED; BROWN, Alan, Daniel; RAWSON, David, James; STORER, Robert, Ian; SWAIN, Nigel, Alan; WO2012/7868; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 13918-92-8, 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. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 4.00 g (21.4 mmol) C-3, 4.3 mL (32 mmol) 2,4-difluorobenzenesulfonyl chloride, 5.2 mL (64 mmol) pyridine and 50 mL DCM is stirred at RT for 5 h. After completion of the reaction, the solvent is removed under reduced pressure, the crude product is taken up in 50 mL water and extracted twice with 100 mL DCM. The combined organic layers are dried over MgSO4 and the solvent is removed under reduced pressure. The crude product can be used without further purification. Yield: 7.88 g (91%).

The chemical industry reduces the impact on the environment during synthesis 2,4-Difluorobenzene-1-sulfonyl chloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; The designation of the inventor has not yet been filed; EP2546249; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics