Author: Jessica.F

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. 102170-53-6, name is 4-Bromo-5-chloro-2-methoxyaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 4-Bromo-5-chloro-2-methoxyaniline

Preparation of 2-(5-chloro-2-methylbenzoxazol-6-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (4) Preparation of 2-amino-5-bromo-4-chlorophenol (2): To a suspension of 4-bromo-3-chloro-6-methoxyaniline (1) (944 mg, 4 mmol) in 10 ml DCM was added 1 M BBr3 in DCM (8 ml, 8 mmol). The reaction mixture was stirred at r.t. for 2 h, which turned to a brown solution and back to a brown suspension. After quenched with aq. sodium bicarbonate solution, the mixture was extracted with EA. The org. phase was washed with brine, dried over sodium sulfate, concentrated to dryness to give 865 mg 2 as brown solid. Yield: 97.2%, purity>95%.

The synthetic route of 102170-53-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CalciMedica, Inc.; US2012/53210; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 2162-98-3, These common heterocyclic compound, 2162-98-3, name is 1,10-Dichlorodecane, 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.

5.68 g (0.05 M) of 4-chloropyridine was dissolved in 50 mL of dimethylformamide, and 15.63 g (0.025 M) of 1,10-dichlorodecane was separately dissolved in 170 mL of dimethylformamide. The 4-chloropyridine solution And the reflux reaction was carried out at 150 DEG C for 20 hours while slowly dropping at 100 DEG CWhen the thin layer chromatography phase reaction is completed, the reaction is stopped by adding about 20 mL of boiling water while cooling the reaction solution. The resulting solution is cooled to 0 C, made alkaline with 35% sodium hydroxide solution and extracted with dichloromethane doThe organic layer was washed with water and then magnesium sulfate was added to remove the water. The solution was distilled under reduced pressure to remove the solvent. 10.53 g of bis (4-chloropyridin-1 (4H) (Yield: 57.0%)

Statistics shows that 1,10-Dichlorodecane is playing an increasingly important role. we look forward to future research findings about 2162-98-3.

Reference:
Patent; Firson Co.,Ltd; Kim, Dong Jin; Koo, Chang Hwei; Park, Sung Yong; Cho, Ir Hwe; Lee, Sung Bae; Han, Dong Hoon; (12 pag.)KR2017/13425; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 320-60-5, 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. 320-60-5, name is 2,4-Dichloro-1-(trifluoromethyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

65 ml of 1.60 mol/1 of n-butyl lithium was slowly dropwise added at a temperature of from-75 to-65C over a period of 30 minutes to a solution of 14.8 ml of 2,4- dichlorobenzotrifluoride in 350 ml of anhydrous tetrahydrofuran, followed by stirring at-70C for 1 hour. At a temperature of from-75 to-65C, 15.9 ml of trimethyl borate was gradually dropwise added, followed by stirring for a while. Then, an ice bath was removed, and the mixture was stirred for 1 hour while gradually warming it to room temperature. Then, the reaction system was cooled to 0C, and 70 ml of ice water and 80 ml of 2N hydrochloric acid were gradually added with stirring, followed by stirring at room temperature overnight. Extraction with diethyl ether was carried out (300 ml x twice). The organic layers were put together, washed with a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. Suction drying was thoroughly carried. out to obtain 28 g of crude 2,6-dichloro-3-trifluoromethylbenzene boronic acid. This product was used as raw material for the next coupling reaction.

The synthetic route of 2,4-Dichloro-1-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ISHIHARA SANGYO KAISHA, LTD.?; WO2005/44007; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1009102-44-6, 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. 1009102-44-6 name is 1-(4-Chlorophenyl)cyclopropanamine 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.

[00108] To a soution of (E)-3-((3aS,5aR,5bR,7aR,9S> 11 aR, 11 bR, 13aS)-9-hydroxy-1 – isopropyl-5a,5b,8,8,1 1 a-pentamethyl-2-oxo- 3,33,4,5,53,5^6,7,78,8,9,10,11 ,11a,11 b,12,13,13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)acrylic acid (500 mg, 1.007 mmol), 1-(4- chlorophenyl)cyclopropanamine hydrochloride (226 mg, 1.107 mmol) and HATU (765 mg, 2.013 mmol) in Nu,Nu-dimethylformamide (DMF) (2 ml_) stirred at 0C was added DIPEA (0.703 mL, 4.03 mmol) . The reaction mixture was stirred at 20 C for 1 h. The reaction mixture was adjusted pH to 3~4 by 2 M HCI, filtered, and the solid was washed with water (50 mL), solved into DCM, dried over sodium sulfate and evaporated in vacuo to give the crude product. The crude product was washed with petrol ether/EtOAc/DCM (10/1/1) to afford the target product (E)-N-(1-(4-chlorophenyl)cyclopropy)-3- ((3aS,5aR,5bR,7aR,9S, 11 aR, 1 1 bR, 13aS)-9-hydroxy-1 -isopropyl-5a,5b,8,8, 11 a- pentamethyl-2-oxo-3,3a,4, 5, 5a, 5b,6,7,7a,8,9, 10, 11 , 11 a, 1 1 b, 12, 13, 13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)acrylamide (685 mg, 1.007 mmol, 100 %)) as a yellow soild.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(4-Chlorophenyl)cyclopropanamine hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; GLAXOSMITHKLINE LLC; HAN, Nianhe; JOHNS, Brian, A.; TANG, Jun; WO2013/91144; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 102170-53-6, 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. 102170-53-6 name is 4-Bromo-5-chloro-2-methoxyaniline, 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.

Preparation of 2-amino-5-bromo-4-chlorophenol (29): To a suspension of 4-bromo-3-chloro-6-methoxyaniline (28) (944 mg, 4 mmol) in 10 ml DCM was added 1 M BBr3 in DCM (8 ml, 8 mmol). The reaction mixture was stirred at r.t. for 2 h, which turned to a brown solution and back to a brown suspension. After quenched with aq. sodium bicarbonate solution, the mixture was extracted with EA. The org. phase was washed with brine, dried over sodium sulfate, concentrated to dryness to give 865 mg of 29 as a brown solid. Yield: 97.2%, purity>95%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-5-chloro-2-methoxyaniline, and friends who are interested can also refer to it.

Reference:
Patent; CalciMedica, Inc.; US2011/263612; (2011); 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. 69411-05-8, name is 3-Chloro-5-trifluoromethylaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3-Chloro-5-trifluoromethylaniline

To a solution of 3-Chloro-5-trifluoromethyl-aniline (425 mul, 3.1 mmol, 1.03 eq.) in dry THF (15 ml) was added 4-Chloro-3-(trifluoromethyl)-phenylisocyanate (665 mg, 3.0 mmol). After stirring overnight at rt the mixture was diluted with cHexane (100 ml), washed twice with 2 N HCl, once with sat. NaHCO3 and brine (100 ml each) and adsorbed on Celite in vacuo. Flash chromatography on silica with cHexane/TBME (4:1 to 2:1) yielded 952 mg product (76%) as a white powder. 1H NMR (DMSO) delta 9.43 (s, 2H), 8.10 (d, J=2.5 Hz, 1H), 7.84 (m, 2H), 7.69 (dd, J=9.0, 2.5 Hz, 1H), 7.64 (d, J=9.0 Hz, 1H), 7.45 (s). MS (ES-): 414.9.

The synthetic route of 69411-05-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Arpida AG; US2009/23813; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1009102-44-6, 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 1009102-44-6 as follows.

To a solution of (E)-3-((3aS,5aR,5bR,7aR,9S,11aR,11bR,13aS)-9-hydroxy-1- isopropyl-5a,5b,8,8, 11 a-pentamethyl-2-oxo- 3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a, 11b, 12,13, 13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)-2-methylacrylic acid (350 mg, 0.685 mmol), 1-(4- chlorophenyl)cyclopropanamine hydrochloride (154 mg, 0.754 mmol) and HATU (521 mg, 1.371 mmol) in DMF (2 mL) stirred at 0C was added DIPEA (0.479 ml_, 2.74 mmol). The reaction mixture was stirred at 20C for 1h. The reaction mixture was pH adjusted to 3-4 with 2 M HCI and filtered. The solid was washed with water (50 mL), dissolved into DCM, dried over sodium sulfate and evaporated in vacuo to give the crude (E)-N-(1-(4- chlorophenyl)cyclopropyl)-3-((3aS,5aR,5bR,7aR,9S, 11 aR, 11 bR, 13aS)-9-hydroxy-1 – isopropyl-5a,5b,8,8, 11 a-pentamethyl-2-oxo- 3,3a,4,5,5a,5b,6,7,7a,8,9,10,11,11a, 11b, 12,13, 13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)-2-methylacrylamide (650 mg, 0.680 mmol, 99 %) as a yellow solid.

According to the analysis of related databases, 1009102-44-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXOSMITHKLINE LLC; HAN, Nianhe; JOHNS, Brian Alvin; TANG, Jun; WO2013/90683; (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. 454-78-4, name is 2-Bromo-1-chloro-4-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Computed Properties of C7H3BrClF3

Preparation of [2-chloro-5-(trifluoromethyl)phenyl]-(2,6-difluorophenyl)methanone (3a); Anhydrous LiCl (16 mol) is introduced in a 25 ml-Schlenk flask having been rinsed with argon and dried under high vacuum (<1 mbar) at 150-170 C. for 5 minutes. Zinc powder (15 mmol) is added under argon and the flask is three-times evacuated and filled with argon. Then, dry THF (10 ml) is added and the zinc is activated with BrCH2CH2Br (5 mol %) and Me3SiCl (1 mol %). The mixture is heated to 50 C. and then, 2-bromo-1-chloro-4-(trifluoromethyl)benzene (5 mmol) in 2 ml dry THF with an internal standard (n-tetradecane) of about 10% are added, followed by 5 mmol N,N,N',N',N-pentamethyldiethylenetetramine. The insertion reaction is completed after 15 hours (control by use of an GC analysis of reaction aliquots wherein the reaction has proceeded for more than 99%). The solution of bromo-[2-chloro-5-(trifluoromethyl)phenyl] zinc (2.5 mmol, 5.5 ml) is carefully separated from the remaining zinc powder by use of a syringe and transferred into another 10 ml-Schlenk flask having been rinsed with argon. The synthetic route of 454-78-4 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Knochel, Paul; Gavryushin, Andrei; Malakhov, Vladimir; Krasovskiy, Arkady; US2011/84230; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 202865-57-4, A common heterocyclic compound, 202865-57-4, name is 1-Bromo-2,5-dichloro-3-fluorobenzene, molecular formula is C6H2BrCl2F, 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.

Preparation 19 1-Bromo-2,5-dichloro-3-methoxybenzene 1-Bromo-2,5-dichloro-3-fluorobenzene (40 g, 0.16 mol) and sodium methoxide (44.3 g, 0.82 mol) were stirred in methanol (500 ml) at the reflux temperature for 16 hours. The reaction was cooled to ambient temperature then quenched with water (500 ml). The mixture was extracted with diethyl ether (3*300 ml), dried (Na2SO4) and evaporated to afford the product as a white solid (40 g) 1H-NMR (CDCl3): 3.90 (s, 3H), 6.86 (d, 1H), 7.26 (d, 1H). MS m/z 256 [MH]+ GC-MS m/z 256 [MH]+, Rt=4.58 min

The synthetic route of 202865-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Pfizer Limited; US2007/105872; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 22911-21-3, A common heterocyclic compound, 22911-21-3, name is 1-Chloro-4-(trimethoxymethyl)benzene, molecular formula is C10H13ClO3, 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-Chloroisoquinolin-5-amine A mixture of 1-chloro-5-nitroisoquinoline (450 mg, 0.0022 mol), stannous chloride dihydrate (2.4 g, 0.011 mol), and EtOAc (50 mL) was stirred under reflux under an atmosphere of nitrogen for 3 h. After cooling, the mixture was poured into ice-water and basified to pH 10.0 with aq. Na2CO3. The organic phase was separated and the aqueous phase was extracted with EtOAc. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated under vacuum. The residue was purified by column chromatography on silica gel to give the product as a light yellow solid. LC-MS: 3.17 min, 179.2 & 181.2 (M+1).

The synthetic route of 22911-21-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kelly, Michael G.; Kincaid, John; Duncton, Matthew; Sahasrabudhe, Kiran; Janagani, Satyanarayana; Upasani, Ravindra B.; Wu, Guoxian; Fang, Yunfeng; Wei, Zhi-Liang; US2006/194801; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics