Category: chlorides-buliding-blocks

These common heterocyclic compound, 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline, 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. Recommanded Product: 202197-26-0

The 3.2g (12.7mmol) compound (VI compound of formula) and 6.4g (53.7mmol) DMF-DMA was added to 100mL eggplant Bottle, heated to reflux for 1h, evaporated under reduced pressure to remove excess DMF-DMA; glacial acetic acid was added 20mL (349.4mmol) and 3.4g (10.7mmol) 2-amino-5-[5-[[[2-(methanesulfonyl)ethyl]amino]methyl]furan-2-yl]benzonitrile (V), was heated under reflux IH; After the reaction system was cooled to room temperature and poured into 80mL of ice water, suction filtered, the filter cake washed with 80mL of methanol and 80mL of ice water Di, 60 C vacuum drying 8h, give lapatinib (a compound of Formula I) 5.1g (8.8mmol, molar yield of 82.4%, HPLC pure Of 99.3%).

The synthetic route of 3-Chloro-4-((3-fluorobenzyl)oxy)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SHANGHAI ACEBRIGHT PHARMACEUTICAL CO., LTD; DAFENG ACEBRIGHT PHARMACEUTICALS CO., LTD; SHANGHAI ACEBRIGHT PHARMACEUTICALS GROUP CO., LTD.; AN, XIAOXIA; LYU, FENG; YAN, LI; WANG, GUANXING; GAI, HONGTAO; LI, HUICHAO; (12 pag.)CN103896889; (2016); B;,
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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. 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, This compound has unique chemical properties. The synthetic route is as follows., Safety of Methyl 2,2,2-trichloroacetimidate

Step B4-bromo-2-(trichloromethyl)-6-[(trifluoromethyl)oxy]-1H-benzim[00346] A suspension of {2-amino-3-bromo-5-[(trifluoromethyl)oxy]phenyl}amine (2.08 g, 6.76 mmol) in acetic acid (35 mL) was treated with methyl 2,2,2-trichloroacetimidate (1.14 mL, 9.21 mmol), added dropwise via syringe. After stirring at rt overnight, the reaction mixture was diluted with water and extracted with diethyl ether (3x). The combined organic layers were washed with water (2x) and brine (1x), then dried over sodium sulfate and concentrated.Toluene was added and the mixture was concentrated under reduced pressure, then dried under vacuum to afford the title compound (2.54 g, 94%). LCMS: m/z 399 (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 2533-69-9.

Reference:
Patent; GLAXOSMITHKLINE LLC; BANKA, Anna; CATALANO, John G; FANG, Jing; PEAT, Andrew James; TAI, Vincent; TURNER, Elizabeth; WO2011/97491; (2011); A1;,
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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. 2106-04-9, name is 3-Chloro-2-fluoroaniline, A new synthetic method of this compound is introduced below., SDS of cas: 2106-04-9

Process step J+K, After 20 min at 50-60 C 1733 g 3-chloro-2-fluoranilin are added to the mixture. The dropping funnel is rinsed with 2 L acetonitrile. Then 7.8 kg 4 M hydrochloric acid in dioxane are added and the mixture is stirred for 45 mm at 55-80 C. After cooling to 1 C. the precipitate is filtered off and washed with 10 L ethanol. The precipitate is suspended in 40 L ethanol and combined with 290 g 3-chloro-2-fluoroaniline. The suspension is stirred for 45 min at 70-80 C and then for 13 h at RT. The precipitate is filtered off and washed with 10 L ethanol. After drying at 60 C in vacuo 4853 g of product is obtained as the hydrochloride.

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:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; OSTERMEIER, Markus; SIEGER, Peter; WO2014/12859; (2014); A1;,
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Electric Literature of 20850-43-5, 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 20850-43-5 as follows.

General procedure: Suspension of the appropriate 3-amino-1,1-dioxo-1,4,2-benzodithiazine derivative 4a-h (0.5 mmol), anhydrous K2CO3 (1.5 mmol, 0.21 g) and the appropriate alkyl chloride (0.6 mmol) in dry THF (5 ml) was heated at reflux for 20-24 h, then cooled in ice-bath and filtered off. The crude product was suspended in 5 ml of water, heated gently to ca. 50 C; and cooled with vigorous stirring until granular precipitate appeared. Filtering off and washing with cold water and diluted EtOH gave pure potassium salts. 4.5.10 ;N-{2-[(1,3-Benzodioxol-5-yl)methylthio]-4-chloro-5-(4-(4-chlorophenyl)thiazol-2-yl)benzenesulfonyl}cyanamide potassium salt (5n) ;Starting from 4f (0.221 g) and 1,3-benzodioxol-5-ylmethyl chloride (0.102 g). Yield: 0.234 g (76%): m.p. 260-262 C; IR (KBr): nu 2895, 2185, 1635, 1578, 1503, 1488, 1472, 1361, 1285, 1142 cm-1; 1H NMR (500 MHz, DMSO-d6): delta 4.32 (s, 2H, SCH2), 6.00 (s, 2H, OCH2O), 6.87-6.89 (m, 1H, Ar), 6.96-6.97 (m, 1H, Ar), 7.04 (s, 1H, Ar), 7.55-7.57 (m, 2H, Ar), 7.60 (s, 1H, Ar), 8.06-8.08 (m, 2H, Ar), 8.41 (s, 1H, Ar), 8.77 (s, 1H, Ar); Anal. C24H14Cl2KN3O4S3 (C, H, N).

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:
Article; Brozewicz, Kamil; Slawinski, Jaroslaw; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 384 – 394;,
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Application of 6775-78-6, These common heterocyclic compound, 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, 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.

Step 2: Preparation of 3-Bromo-6-chloroimidazo[1,2-b]pyridazine (0530) (0531) 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-bromo-succinimide 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 saturated 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. (0532) 1H-NMR (CHLOROFORM-d): delta [ppm]=7.12 (d, 1H); 7.79 (s, 1H); 7.90, (d, 1H).

The synthetic route of 6775-78-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; SCHULZE, Volker; EIS, Knut; PUEHLER, Florian; ZORN, Ludwig; SUeLZLE, Detlev; LIENAU, Philip; WENGNER, Antje Margret; PETERSEN, Kirstin; BOeMER, Ulf; (68 pag.)US2017/29441; (2017); A1;,
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Application of 57946-56-2, These common heterocyclic compound, 57946-56-2, name is 4-Chloro-2-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 solution of 4-chloro-2-fluoroaniline (50.0 g, 344 mmol) in AcOH (3OmL) is added Ac2O (60 ml_) and the reaction is stirred at room temperature for 2 hours. The mixture is poured into ice water (500 mL) to give a solid precipitate. The mixture is stirred for an additional 1 hour at room temperature. The solid is filtered and washed with water and hexanes, then air dried to give lambda/-(4-chloro-2-fluorophenyl) acetamide

The synthetic route of 57946-56-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GmbH; WO2008/2853; (2008); A2;,
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. 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine, A new synthetic method of this compound is introduced below., Application In Synthesis of 4-Chloro-5-fluorobenzene-1,2-diamine

General procedure: A mixture of compounds 1a-l (0.013 mol) and 4-chloro-5-fluoro-ophenylenediamine(2) (0.01 mol) in methanol (10 mL) was irradiatedwith ultrasonic irradiation at 50 C for 7 min (8 min for 3a) Afterreaction completion (monitored by TLC, ethyl acetate/hexane = 3:1), themixture was poured onto water and the precipitated product was filtrated off, washed with water and recrystallised from ethanol/water, 3:1.

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

Reference:
Article; Mente?e, Emre; Kahveci, Bahittin; Mente?e, Meltem; Journal of Chemical Research; vol. 42; 6; (2018); p. 329 – 331;,
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Application of 13726-14-2, A common heterocyclic compound, 13726-14-2, name is 4-Chloro-3-methoxyaniline, molecular formula is C7H8ClNO, 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 solution of compound 5 (15 mg, 0.037 mmol) in DMF (3 mL)4-Chloro-3-methoxyaniline (6.2 mg, 0.04 mmol) was added.HATU (17 mg, 0.045 mmol) and TEA (7.5 mg, 0.074 mmol),Stir at room temperature for 2 hours,It was poured into water (10 mL) and extracted with ethyl acetate (2×5 mL).The organic phase was separated and washed with saturated aqueous NaCI (2×).The organic phase was separated and dried over anhydrous Na2SO4, filtered and concentrated.The residue was purified by silica gel column chromatography.Elution with ethyl acetate/petroleum ether (1:2) gave the desired compound I-8 (11 mg, 55%).

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

Reference:
Patent; Nanjing Gentai Pharmaceutical Co., Ltd.; Chen Rongyao; Shen Yu; (48 pag.)CN110218182; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2106-04-9, name is 3-Chloro-2-fluoroaniline, 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 2106-04-9, Recommanded Product: 2106-04-9

Intermediate 32A. Ethyl 3-((3-chloro-2-fluorophenyl)amino)-2-nitrobut-2-enoate: Using a modified procedure described by Gomez-Sanchez. (Reference: Gomez-Sanchez, A. et al, Anales De Quimica, 81(2): 139 (1985)) A clear, faint yellow solution of ethyl nitroacetate (4.17 mL, 37.6 mmol) and triethylorthoacetate (6.93 mL, 37.6 mmol) in toluene (9.39 mL) was heated to 1 10 C. A Dean-Stark trap was used to azeotrope the ethanol. Approximately every 30 min, the solvent was removed from the Dean-Stark and additional toluene (6 mL) was added to the reaction flask. Over the course of the reaction the color became a clear, dull yellow color. After 7.5 h, the reaction was stopped and it was cooled to room temperature. Excess solvent and starting materials were removed by distillation (5 mm Hg at 100 C) leaving ethyl 3-ethoxy-2-nitrobut-2-enoate (5.46 g) as an orange liquid. An orange solution of 3-chloro-2-fluoroaniline (5.86 g, 40.2 mmol) and ethyl 3-ethoxy-2-nitrobut-2-enoate (5.45 g, 26.8 mmol) in ethanol (13.41 mL) was stirred at room temperature. After 7 h, the reaction was stopped and concentrated to give an orange oil. The orange oil was diluted with EtOAc and washed with 1.0 N HC1 (2*), saturated aHC03, brine, dried over sodium sulfate, filtered and concentrated to give an orange oil. Purification by normal phase chromatography gave Intermediate 32A (2.90 g, 36%) as a viscous orange-yellow oil. XH NMR indicated a 1 : 1 E:Z mixture. MS (ESI) m/z: 325.0 (M+H)+.

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Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; PINTO, Donald J.P.; CLARK, Charles G.; SMITH, II, Leon M.; ORWAT, Michael J.; JEON, Yoon; CORTE, James R.; WO2014/160668; (2014); 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. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1-(2-Chloroethyl)azepane hydrochloride

To a solution of 1,1-bis(4-hydroxyphenyl)ethane (50.0 mg, 0.233 mmol) in DMF (2.33 mL) at 0 °C was added 60percent sodium hydride (dispersion in paraffin liquid, 56.0 mg, 1.40 mmol). The reaction mixture was stirred for 15 min at 50 °C and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (153 mg, 0.772 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 23 h at 50 °C, saturated aqueous ammonium chloride was added at 0 °C. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 30/1) to afford RID-F-S*101 (compound 26) (93.9 mg, 87percent) asa pale yellow oil

The synthetic route of 26487-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
Chloride – Wikipedia,
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