Category: chlorides-buliding-blocks

Some common heterocyclic compound, 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, molecular formula is C8H9ClO4S, 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. Recommanded Product: 63624-28-2

General procedure: A solution of the appropriate acid halide fragments (4.8 mmol)in dry pyridine (5 mL) was dropwise added to a well-stirredmixture of the intermediate 3-amino-substituted rutaecarpine 5(4 mmol) in dry pyridine (50 mL) at room temperature. The reactionwasstirred for 30 min and monitored by TLC. After the reactioncompleted, the pH was adjusted to neutral with dilute hydrochloricacid. The pyridine and residual sulfonyl chloride were distilledunder reduced pressure. The mixture was extracted with an ethylacetate-water system. The aqueous layer was discarded and ethyl acetate was evaporated to obtain crude product. The crude productwas washed with water and dried under vacuum. The solid residuewas purified by flash chromatography on silica gel with ethyl acetate/petroleum ether (1:1) elution to provide the desired derivatives6a-6p, 7a-7c, and 8a.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 63624-28-2, its application will become more common.

Reference:
Article; Wu, Mingfei; Ma, Jie; Ji, Lijun; Wang, Min; Han, Jianfei; Li, Zeng; European Journal of Medicinal Chemistry; vol. 177; (2019); p. 198 – 211;,
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Some common heterocyclic compound, 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, molecular formula is C6H4ClN3, 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. Computed Properties of C6H4ClN3

Step 2: Preparation of 3-Bromo-6-chloroimidazo[1,2-b]pyridazine 478 mg (3.11 mmol) of 6-chloroimidazo[1,2-b]pyridazine were introduced into 10 mL of chloroform under argon and, while cooling in ice, 664 mg (3.73 mmol) of N-bromosuccuinimide were added. After the addition was complete, the reaction mixture was stirred at room temperature overnight. The reaction mixture was then mixed with water and ethyl acetate and, after addition of saturated sodium bicarbonate solution, the phases were separated. The aqueous phase was extracted three more times with ethyl acetate. The combined organic phases were then washed with sat. sodium chloride solution and dried over sodium sulfate. In the final removal of the solvent in vacuo, the desired product was isolated in quantitative yield in the form of an amorphous white solid which was employed without further chromatographic purification in subsequent reactions. 1H-NMR (CHLOROFORM-d): delta [ppm]=7.12 (1H); 7.79 (1H); 7.90 (1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6775-78-6, its application will become more common.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; Eis, Knut; Puehler, Florian; Zorn, Ludwig; Schulze, Volker; Suelzle, Detlev; Lienau, Philip; Haegebarth, Andrea; Petersen, Kirstin; Boemer, Ulf; US2015/87631; (2015); A1;,
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Related Products of 210532-25-5, 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. 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows.

Example llbis-a: N-(6-chloro-5-cyanopyridin-3-yl)-3,5-difluorobenzene- sulfonamide 1.132 g (5.32 mmol) of 3,5-difluorobenzene-l-sulfonyle chloride is added under argon to a solution of 545 mg (3.55 mmol) of 5-amino-2-chloronicotinotrile in 20 mL of an anhydrous 1 : 1 mixture of THF and pyridine. The reaction medium is heated to 70C for 3 hours and let 12 additional hours under stirring at room temperature. The solvent is dry evaporated and the crude reaction product is redissolved in ethyl acetate and washed with several aqueous fractions. The organic phase is dried on magnesium sulfate, filtered, concentrated and then purified by silica gel chromatography to yield 784 mg (67%) of N-(6-chloro-5-cyanopyridin-3-yl)-3,5-difluorobenzene-sulfonamide. 1H NMR: deltaEta ppm (400 MHz, DMSO): 11 ,39 (1H, si, NH), 8.34 (1H, m, CHarom), 8.10 (1H, m, CHarom), 7.67 (1H, m, CHarom), 7.59 (2H, m, CHarom).

The chemical industry reduces the impact on the environment during synthesis 3,5-Difluorobenzene-1-sulfonyl chloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; PIERRE FABRE MEDICAMENT; SOKOLOFF, Pierre; CACHOUX, Frederic; WO2014/16433; (2014); A1;,
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Reference of 57946-56-2,Some common heterocyclic compound, 57946-56-2, name is 4-Chloro-2-fluoroaniline, molecular formula is C6H5ClFN, 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.

To a solution of 4-chloro-2-fluoroaniline (1.15 g, 7.9 mmol) in 125 mL of ethanol added silver sulphate (1.7 g, 8.3 mmol), then followed by addition of I2 (2.1 g, 8.3 mmol) in portions. After the addition was completed, the mixture was stirred at RT for 2 hours. The mixture was filtered through celite and the filtration was evaporated to give dark oil which was dissolved in 125 mL of DCM. The solution was washed with 2M sodium hydroxide (40 mL×2), saturated Na2S2O3 (40 mL×2) and water (40 mL×2). The resulting solution was dried over MgSO4 and then evaporated to give the crude 4-chloro-2-fluoro-6-iodoaniline as dark oil (2.1 g, yield: 98%).

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

Reference:
Patent; Hoffmann-La Roche Inc.; FENG, Song; GAO, LU; HONG, Di; WANG, Lisha; YUN, Hongying; ZHAO, Shu-Hai; (89 pag.)US2016/200741; (2016); A1;,
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Reference of 2687-12-9, 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. 2687-12-9 name is Cinnamyl chloride, 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.

General procedure: A representative procedure of skeleton 4 is as follows: K2CO3 (400 mg, 2.9 mmol) was added to a solution of 3 (1.0 mmol) in acetone (10 mL) at rt. The reaction mixture was stirred at rt for 10 min. Cinnamyl chloride (1.05 mmol) was added to the reaction mixture at rt. The reaction mixture was stirred at reflux for 8 h. The reaction mixture was cooled to rt, concentrated, and extracted with CH2Cl2 (3×20 mL). The combined organic layers were washed with brine, dried, filtered, and evaporated to afford crude product under reduced pressure. Purification on silica gel (hexanes/EtOAc=6:1 to 1:1) afforded 4.

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

Reference:
Article; Chang, Meng-Yang; Lu, Yi-Ju; Cheng, Yu-Chieh; Tetrahedron; vol. 71; 8; (2015); p. 1192 – 1201;,
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Adding a certain compound to certain chemical reactions, such as: 13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine, 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 13745-86-3, category: chlorides-buliding-blocks

Combine 11-chloro-dibenzo[b,f][1, 4] thiazepine (700 mg), 2- (R)-BENZYL-PIPERAZINE (1.0 g) and toluene (10 mL), heat to reflux for 19 hours, then cool down to ambient temperature. Concentrate and purify by flash chromatography (dichloromethane then gradient of methanol 3-10%) to give the title compound as a white solid (734 mg, 74%): mp 56-69 C ; LHNMR (CDCI3) O2. 58 (dd, 1H), 3.18-2. 60 (M, 6H), 6.88 (dt, 1H), 7.07 (dd, 1H), 7.34-7. 14 (m, 9H), 7.39 (dd, 1H), 7.53-7. 47 (m, 1H) ; MS (APCI) N7LZ (rel intensity) 386.4 (100).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 11-Chlorodibenzo[b,f][1,4]thiazepine, and friends who are interested can also refer to it.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/26177; (2005); A1;,
Chloride – Wikipedia,
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Electric Literature of 2729-34-2, These common heterocyclic compound, 2729-34-2, name is 3,5-Dichloro-4-fluoroaniline, 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.

To a cooled (-20 C) solution of (R)-2-tert-butoxycarbonylamino-propionic acid (57.2 g, 302 mmol) in anhydrous THF (582 mL) was added JV-methyl-morpholine (34.9 mL, 317 mmol) at a rate to keep the internal temperature at -15 C. Isobutyl chloroformate (42.0 mL, 317 mmol) was then added over a 20 min period and the resulting mixture was stirred for 30 min. A solution of 3,5-dichloro-4-fluoro-phenylamine (54.4 g, 302 mmol) in THF (160 mL) was then added over 40 min. The reaction mixture was warmed to 20 C and stirred for 20 h. The reaction mixture was filtered and concentrated in vacuo. To the resulting oil was added MeOH (200 mL) and the solution was concentrated to provide the title compound as a tan colored solid, m/z 295.3 [M-?-Bu]+. This material was used without further purification.

Statistics shows that 3,5-Dichloro-4-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 2729-34-2.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO. KG; WO2009/70485; (2009); A1;,
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. 13726-14-2, name is 4-Chloro-3-methoxyaniline, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

A mixture of substituted 2,4-dichloropyrimidine (1.0 equiv.), and substituted aniline (1.0-1.05 equiv.), and DIPEA (1.2 equiv.) in isopropanol (0.1 M) was stirred and heated at reflux. The reaction time, work-up, and product isolation procedure are described below. 2,5-Dichloro-/Y4-(4-chloro-3-methoxyphenyl)pyrimidin-4-amine (SG1-168): This was prepared from 2,4,5-trichloropyrimidine (0.500 g), 4-chloro-3-methoxyaniline (0.451 g), and DIPEA (0.570 mL) using procedure B (reaction time, 12 h). The solvent was removed and EtOAc (20 mL) was added. The organic layer was extracted with water (20 mL). The aqueous layer was re-extracted with EtOAc (20 mL). The organic layers were combined and washed with water and brine (20 mL each), dried (Na2S04) and concentrated under reduced pressure. The resulting dark purple oil was triturated using EtOAc/hexanes to give the title compound as a light purple solid (0.680 g, 82%). Mp: 136-138 C. NMR (400 MHz, DMSO-ifc): delta 9.57 (s, 1H, disappeared on D20 shake), 8.41 (s, 1H), 7.49 (d, / = 2.2 Hz, 1H), 7.41 (d, / = 8.6 Hz, 1H), 7.28 (dd, / = 8.6, 2.2 Hz, 1H), 3.82 (s, 3H). HPLC-MS (ESI+): m/z 308.1 [40%, (M35C137C137C1+H)+], 306.1 [98%, (M35C135C137C1+H)+], 304.0 [100%, (M35C135C135C1+H)+].

The synthetic route of 13726-14-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; H. LEE MOFFITT CANCER CENTER & RESEARCH INSTITUTE, INC.; SCHOeNBRUNN, Ernst; LAWRENCE, Nicholas J.; LAWRENCE, Harshani R.; (293 pag.)WO2017/66428; (2017); A1;,
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. 64628-73-5, name is 3-Chloro-4-(trifluoromethoxy)aniline, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H5ClF3NO

Reference Example 24 A solution of 3-chloro4-trifluoromethoxyaniline (5.1 g) in acetic acid (31 ml) was stirred and treated with sodium nitrite (2.16 g) in concentrated sulphuric acid (14 ml) at below 18 C. After an additional 1 hour at 10 C., the solution was added to a mixture of copper (I) bromide (7.7 g) and hydrobromic acid (24.5 ml) in water at 40-50 C. The reaction was completed by heating at 50 C. for 2 hours, water was added and the mixture filtered. The filtrate was extracted with ether, washed with sodium bicarbonate, dried (magnesium sulphate) and evaporated to give 3-chloro-4-trifluoromethoxy-bromobenzene (6.05 g) as a brown oil, NMR (CDCl3) 7.10(m,1H), 7.35(m,1H), 7.55(d,1H). By proceeding in a similar manner 2-nitro-4-trifluoromethoxy-bromobenzene was prepared, NMR (CDCl3) 7.35(m,1H), 7.75(m,1H), 7.8(d,1H).

According to the analysis of related databases, 64628-73-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Rhone-Poulenc Agriculture Limited; US6323155; (2001); B1;,
Chloride – Wikipedia,
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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. 886762-39-6, name is 3,4-Dichloro-2-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 3,4-Dichloro-2-fluoroaniline

1 .43 g of the compound obtained in (1-5), 1 .91 g of (R)-(-)-N-Boc-4- hydroxypiperidine and 1 .96 g of triphenylphosphine were added to 20 ml of methylene chloride, and 2.01 ml of diisopropylazodicarboxylate was added thereto dropwise. The resulting mixture was stirred at room temperature for 1 hour and distilled under a reduced pressure, and the residue was briefly purified by columnchromatography (ethylacetate : methylenechloride : methanol = 20 :20: 1). The partially purified residue was then dissolved in 60 ml of 2-propanol, 1 .17 g of 3,4- dichloro-4-fluoroaniline was thereto, and the mixture was stirred at 1 00 00 for 3 hours. The resulting mixture was distilled under a reduced pressure to remove the solvent, and the residue was dissolved in 60 ml of methylenechloride. 60 ml oftrifluoroacetic acid was added thereto and the mixture was stirred at room temperature for 1 hour. The resulting mixture was distilled under a reduced pressure to remove the solvent. Saturated sodium bicarbonate solution was added to the resulting residue to make it basic, followed by extraction with chloroform. The organic layer was dried over anhydrous sodium sulfate, filtered, and distilled under a reduced pressure. The resulting residue was subjected to column chromatography (chloroform : methanol = 1: 2) to obtain the title compound.

The synthetic route of 886762-39-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SPECTRUM PHARMACEUTICALS, INC.; CHATURVEDUAL, Prasad, V.; KOLLI, Prasad; (46 pag.)WO2019/79599; (2019); A1;,
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