Tag: M.W=200-300

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. 18282-59-2, name is 4-Bromo-1,2-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 18282-59-2

A solution of 1-bromo-3,4-dichlorobenzene (16.92 g, 0.074 mol) in Et2O (100 ml) was added to a suspension of magnesium turnings in Et2O (60 ml) and the mixture was refluxed for 1 hour. The reaction was cooled to 23¡ã C. and a solution of 4-cyanopyridine 54 (7.80 g, 0.075 mol) in 1:1 Et2O:THF (150 ml) was added rapidly with vigorous stirring. The mixture was refluxed for 24 h, then cooled to 23¡ã C. Ice (100 g) was added, followed by 50percent H2SO4 (50 ml), and the mixture was stirred for 1 h. Et2O (100 ml) was added, the aqueous layer was separated, made basic with 10percent NaOH, and extracted with EtOAc (2.x.250 ml). The combined organic layer was dried (Na2SO4), filtered, and concentrated. Purification by silica gel chromatography (eluant: 30percent EtOAc: CH2Cl2) gave 12 g (0.047 mol, 64percent) of the product 55 as a colorless oil. MS (FAB for M+1): m/e 252.

According to the analysis of related databases, 18282-59-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SCHERING CORPORATION; US2005/182095; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 202197-26-0, 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.

3) 1.20 g (5.7 mmol) of 4-chloro-6-nitro-quinazoline and 1.37 g (5.6 mmol) of 4-(3-fluoro-benzyloxy)-3-chloro-aniline were dissolved in 80 mL of isopropanol and refluxed for 3 hours. A large amount of yellow solid precipitated from the system. The solid was collected by filtration, washed with saturated sodium bicarbonate solution till pH=8 and dried under vacuum to obtain 1.62 g (3.75 mmol) of yellow solid, which was identified as the compound 4-[3-chloro-4-(3-fluoro-benzyloxy)phenylamino]-6-nitro-quinazoline with a yield of 67%.1H-NMR (400 MHz, CDCl3): delta11.30 (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; Guo, Jianhui; Jiang, Yong; US2010/168142; (2010); 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. 16793-91-2, name is 2-Chlorophenethyl Bromide, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Chlorophenethyl Bromide

Example 14: Preparation of 8-r2-(2-chlorophenyl)ethvn-3-methyl-4-((4-r3- (trifluoromethyl)phenynpiperazin-1-yl>carbonyl)-1-oxa-8-azaspiror4.51dec-3-en-2-oneA mixture of 3-methyl-4-({4-[3-(trifluoromethyl)phenyl]piperazin-1-yl}carbonyl)-1 -oxa-8- azaspiro[4.5]dec-3-en-2-one dihydrochloride (Example 1 , 200 mg, 0.40 mmol), anhydrous potassium carbonate (180 mg, 1.30 mmol) and 1-(2-bromo-ethyl)-2-chloro-benzene (0.07 mL, 0.22 mmol) in anhydrous N.N-dimethylformamide (3 mL) was heated at 90C for 1.5 hours under microwave irradiation. The reaction mixture was concentrated under vacuum. The residue was taken up in dichloromethane (20 mL), washed with water (20 mL) and brine (20 mL), dried (MgS0 ) and concentrated under vacuum. After purification by flash chromatography (silica), the title compound was obtained as a white solid. 1H NMR (DMSO-d6, 400 MHz): delta 7.46-7.34 (m, 3H), 7.26-7.23 (m, 4H), 7.11 (d, J = 7.5 Hz, 1 H), 3.80-3.79 (m, 1 H), 3.68-3.69 (m, 1 H), 3.56 (s, 2H), 3.27 (s, 1 H), 3.16-3.15 (m, 2H), 2.93-2.92 (m, 1 H), 2.87-2.83 (m, 4H), 2.53 (s, 2H), 2.25-2.24 (m, 3H), 1.88-1.87 (m, 1 H), 1.76 (s, 3H), 1.72 (s, 1 H), 1.52 (s, 1 H). LCMS (Method D): Mass found (M+ 562), Rt (min): 4.64, Area (%): 99.5 (Max), 99.6 (254 nm). HPLC (Method A): Rt (min): 4.61 , Area (%): 98.5 (Max), 99.3 (254 nm).

According to the analysis of related databases, 16793-91-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ARES TRADING S.A.; JORAND-LEBRUN, Catherine; SWINNEN, Dominique; GERBER, Patrick; KULKARNI, Santosh; WO2012/130915; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 328-84-7, 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. 328-84-7, name is 3,4-Dichlorobenzotrifluoride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 1 Synthesis of 2,3-dichloro-6-trifluoromethylbenzaldehyde STR10 54 g (0.25 mol) of 3,4-dichlorobenzotrifluoride was dissolved in 500 ml of anhydrous THF, and cooled down to -70 C. with dry ice/acetone. To the solution, 190 ml (0.3 mol) of hexane solution of n-butyl lithium was added dropwise over 45 minutes, while keeping the temperature at -70 C. The reaction solution was matured for an hour at -70 C., then 30 g (0.5 mol) of methyl formate was dropped into the solution over 30 minutes, while keeping the temperature at -70 C. After the reaction solution was matured for an hour at -70 C., the temperature of the solution was elevated to room temperature. The reaction solution was poured into ice water and extracted with ether. The organic layer obtained was washed with water and then dried over anhydrous magnesium sulfate. The solvent was distilled out under reduced pressure. The resulting residue was distilled to give 47.3 g of oily product. Yield 77% (purity 95%), 84~94 C./3mmHg.

The synthetic route of 3,4-Dichlorobenzotrifluoride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nippon Soda Co., Ltd.; US5977414; (1999); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route 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.

To a solution of 3,5-difluorobenzenesulfonyl chloride (25 g, 0.117 mol) in THF (150 mL) was added 35% aq. NH4OH (120 mL) over 1 h in an ice-bath. After the reaction was complete, it was evaporated in vacuo. To a solution of this residue in water (150 mL) was added 2N HC1 (1 mL). After stirring 1 h, the reaction mixture was filtered and dried under high vacuum to give 3,5-difluorobenzenesulfonamide as a light brown solid (19.9 g, 88%). 1H NMR (400MHz, CDC13) delta 7.49-7.44 (m, 2H), 7.04-6.99 (m, 2H).

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; EXELIXIS, INC.; BOLLU, Venkataiah; BOREN, Brant, Clayton; DALGARD, Jackline; FLATT, Brenton, T.; HAQ, Nadia; HUDSON, Sarah; MOHAN, Raju; MORRISSEY, Michael; PRATT, Benjamin; WO2011/71565; (2011); 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. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-2-chloro-1-fluorobenzene

Example 112 Production of (4aS, 8aR)- 1 -(3 -chloro-4-fluoropheny l)-3 , 3 -dimethy ldecahydroquinoxaline hydrochloride bsolute configuration A toluene (10 ml) suspension of (4aR,8aS)-2,2-dimethyldecahydroquinoxaline (168 mg, 0.998 mmol), 4-bromo-2-chloro-l-fluorobenzene (251 mg, 1.20 mmol), Pd(OAc)2 (11.2 mg, 0.0500 mmol), t-Bu3P.HBF4 (14.5 mg, 0.0500 mmol), and NaOt-Bu (135 mg, 1.40 mmol) was stirred for 5 hours under reflux in a nitrogen atmosphere. The reaction solution was cooled to room temperature. Then, water (0.5 mL) and AcOEt (10 mL) were added thereto, and the mixture was stirred. MgS04 was further added thereto, and the mixture was stirred. Then, insoluble matter was filtered. The filtrate was concentrated under reduced pressure, and the obtained residue was purified by basic silica gel column chromatography (Hex- AcOEt). The obtained oil was dissolved in 1 N HCl-EtOH (3 mL), and ethanol was distilled off under reduced pressure. The deposited crystal was recrystallized from ethanol/acetone to obtain (4aS,8aR)-l- (3-chloro-4-fluorophenyl)-3,3-dimethyldecahydroquinoxaline hydrochloride (153 mg, yield: 46%) in a white powder form. 1H-NMR ( DMSO-de ) 6ppm : 1.15-1.45 ( 6H, m ), 1.51 ( 3H, s ), 1.6-1.9 ( 4H, m ), 1.9-2.05 ( 1H, m ), 2.94 ( 1H, d, J = 13.5Hz ), 3.3-3.45 ( lH, m ), 3.65-3.8 ( 1H, m ), 3.95-4.1 ( 1H, m ), 6.85-7.0 ( 1H, m ), 7.12 ( 1H, dd, J = 3.0, 6.2Hz ), 7.25 ( 1H, dd, J = 9.1, 9. lHz ), 8.13 ( 1H, br ), 9.86 ( 1H, br ).

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; OTSUKA PHARMACEUTICAL CO., LTD.; SHINOHARA, Tomoichi; SASAKI, Hirofumi; TAI, Kuninori; ITO, Nobuaki; WO2013/137479; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 41965-95-1, 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. 41965-95-1 name is 3-Chloro-4-methoxybenzylamine Hydrochloride, 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.

To a heterogenous mixture of quinoline 13 (3.56 mmol) and 3-chloro-4- methoxy benzylamine-HCl (3.92 mmol) in NMP (15 mL) was added TNEt (8.90 mmol). The reaction mixture was heated to 80 C for 3 h. Subsequently, cooled the reaction mixture to ambient temperature and added 1M aqueous HQ and EtOAc. The resulting layers were separated and the organic layer washed with water (3x) followed by brine (1 x). The combined organic layers were dried over Na2S04, filtered, and concentrated in vacuo. The residue was dissolved in a minimum amount of hot EtOAc and allowed to cool to ambient temperature. Hexanes was then added to the solution and the intermediate 14 (80% yield) precipitated out and was collected by vacuum filtration. H NMR (300 MHz, CDCIj) 8 8.20 (s, 1 H), 7.95 (d, I H, , 7-8.4 Hz), 7.82 (d, 1 J=7.5 Hz), 7.38 is, IB), 7.27-7.22 im, 1 H), 6.98 (d, IR , 7-8.4 Hz), 6.26 (s, 1H), 4.54 (d. 2H J-4.8 Hz), 3.95 (s, 3H), 3.93 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-4-methoxybenzylamine Hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; LANDRY, Donald, W.; DENG, Shixian; ARANCIO, Ottavio; FIORITO, Joie; WASMUTH, Andrew; WO2013/109738; (2013); 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. 699-89-8, name is 4,7-Dichlorothieno[2,3-d]pyridazine, A new synthetic method of this compound is introduced below., Recommanded Product: 699-89-8

Equal equivalents of dichloride (1) and M-NH2 are refluxed in the appropriate amount of absolute ethanol at 95 0C for 2 hrs. The reaction mixture is allowed to cool to room temperature and the precipitate (2) that forms is filtered and washed sequentially with isopropyl alcohol, 4.0 N KOH, H2O, and hexane, and then dried. The filtrate (2) is then reacted with 1.2 equivalent Of Q-NH2 in an appropriate amount of n-butyl alcohol at 150 0C for 10 hrs. The reaction is cooled to room temperature before the solvent is evaporated under reduced pressure. The residue is treated with aqueous 4.0 NKOH solution and extracted with dichloromethane. The organic layer is dried (MgSO4) and evaporated. The crude product (3) is purified by preparative thin layer chromatography (TLC) or flash chromatography on silica gel using dichloromethane/methanol (95:5) as the eluent. Final product is confirmed by LC/MS and/or nuMR. The invention compounds of Examples 23 – 25, 48, and 76-80 as shown in the below table were prepared by method A-I.

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; BAYER HEALTHCARE AG; WO2007/118602; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 19752-55-7 as follows. Product Details of 19752-55-7

In a 20 mL eggplant flask, 3,3′-bicarbazole,1-Bromo-3,5-dichlorobenzene, copper powder, potassium carbonate and nitrobenzene were charged, nitrogen bubbling was carried out for 1 hour, and the mixture was stirred at 170 C. for 17 hours under a nitrogen stream. Progress of the reaction was confirmed by TLC (ethyl acetate: hexane = 1: 3) to confirm disappearance of 3,3′-bicarbazole and cooled to room temperature. The reaction mixture was dissolved in chloroform and the insoluble matter was filtered through celite. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform: hexane = 1: 1) to obtain a pale yellow solid of BCzPhCl (yield: 810 mg, yield: 54%). It was identified by mass spectrometry (MS), 1 H-NMR. A chart of 1 H-NMR is shown in FIG. 2, and an enlarged view thereof is shown in FIG. 3. Table 1 shows the preparation conditions of this synthesis.A similar experiment is shown in Table 1Run No. 2

According to the analysis of related databases, 19752-55-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ChemiprokaseiCo., Ltd.; Kido Junji, Sasabe; Hisahiro, Naoki; Toyota, Naoki; Omae, Yoshinori; (110 pag.)JP5727237; (2015); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 823-57-4,Some common heterocyclic compound, 823-57-4, name is 2-Bromo-5-chloroaniline, molecular formula is C6H5BrClN, 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.

Compound 16-3 (0417) A solution of 16-2 (3.778 g, 18.43 mmol), Bis(pinacolato)diboron (8.5 g, 33.17 mol), KOAc (3.2 g, 36.86 mmol) and Pd(dppf)2Cl2DCM (500 mg, 0.92 mmol) in DMSO (50 mL) was stirred at 85¡ã C. for 2.5 h. TLC showed that the reaction was complete. Water (60 mL) was added and the mixture was extracted with ethyl acetate (60 mL¡Á3). The combined organic layers were dried over Na2SO4, filtered, concentrated and purified by silica gel column (PE:EA=10:1) to afford 16-3 as a yellow solid (5.0 g, yield 100percent).

The synthetic route of 823-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nivalis Therapeutics, Inc.; Wasley, Jan; Rosenthal, Gary J.; Sun, Xicheng; Strong, Sarah; Qiu, Jian; US9138427; (2015); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics