Tag: M.W=200-300

Reference of 16429-44-0, A common heterocyclic compound, 16429-44-0, name is 5-Bromo-3-chlorobenzene-1,2-diamine, molecular formula is C6H6BrClN2, 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.

General procedure for the synthesis of U3A mixture of U2 (7.2 g, 32.5 mmol) and CDI (6.32 g, 39.0 mmol) in anhydrous THF (100 mL) was refluxed for 16 hours. After cooling to room temperature, the white precipitate was collected by filtration and dried under reduced pressure to afford U3.

The synthetic route of 16429-44-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INSTITUT PASTEUR KOREA; QURIENT CO., LTD.; KIM, Jaeseung; AHN, Seohyun; JEON, Yeejin; PARK, Dongsik; YANG, Young-In; LEE, Doohyung; LEE, SaeYeon; AHN, Jiye; KIM, Jeongjun; NAM, Kiyean; KANG, Sunhee; SEO, MinJung; SEO, Mooyoung; SEO, Jeongjea; HAN, Sung-Jun; KIM, Jung Hwan; LEE, Sangchul; CHOI, Gahee; LEE, Yunmi; (184 pag.)WO2016/16421; (2016); 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. 59772-49-5, name is 2-Bromo-6-chloroaniline, A new synthetic method of this compound is introduced below., Safety of 2-Bromo-6-chloroaniline

Benzo [b] thiophen-3-ylboronic acid (162 g, 1000 mmol),2-bromo-6-chloroaniline (189 g, 1100 mmol) was dissolved in toluene (toluene) (Pd (PPh3) 4 (58 g, 50 mmol) was dissolved in 400 mL of EtOH,NaHCO3 (252 g, 3000 mmol) was added thereto and refluxed for 4 hours.After completion of reaction, MC is extracted by cooling to room temperature.After drying over anhydrous MgSO4, the solvent is removed by rotary evaporator. Column chromatography (MC: Hx = 1: 3) was used to obtain the desired compound 1-5. (190 g, 91percent, brown oil)

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; L Ti Material Co., Ltd.; Oh Han-guk; Lee Yun-ji; Ji Hye-su; Jeong Won-jang; Choi Jin-seok; Choi Dae-hyeok; (212 pag.)KR2019/33885; (2019); A;,
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Application of 208186-78-1, 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. 208186-78-1, name is 1,2-Dibromo-5-chloro-3-fluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Step 1: Slowly add isopropyl to a mixture of 1,2-dibromo-5-chloro-3-fluorobenzene (5 g, 17.5 mmol) in n-hexane (12 mL) and tetrahydrofuran (20 mL) at -45C. A solution of magnesium chloride in tetrahydrofuran (19.2 mol, 1 M) was maintained at a temperature of -40C. DMF (6.4 g, 87.5 mmol) was then slowly added dropwise to the above reaction mixture and stirred for 30 minutes. The reaction system was prepared with hydrochloric acid (15 mL, 2.0M) Quenching.The mixture was warmed to room temperature and diluted with ethyl acetate (80 mL) and the organic phase was separated.The organic phase was washed with saturated brine, filtered, and the filtrate was concentrated under reduced pressure.The residue was purified by flash column chromatography (petroleum ether/ethyl acetate = 10/1) to give 2-bromo-4-chloro-6-fluorobenzaldehyde (3 g, yield: 73%) as a yellow solid.

The chemical industry reduces the impact on the environment during synthesis 1,2-Dibromo-5-chloro-3-fluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Shanghai Dinuo Pharmaceutical Technology Co., Ltd.; Li Qun; Liu Shengyang; (54 pag.)CN107556244; (2018); A;,
Chloride – Wikipedia,
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Application of 909122-17-4, 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. 909122-17-4 name is 1-Bromo-2-chloro-4-ethoxy-3-fluorobenzene, 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.

First Step 1.0 g of well dried magnesium and 30 mL of THF were placed in a reactor under nitrogen atmosphere, and heated to 43° C. 10.0 g of 1-bromo-2-chloro-4-ethoxy-3-fluorobenzene (6) dissolved in 20 mL of THF was slowly added dropwise thereto at a temperature range of from 43 to 51° C., followed by stirring for 30 minutes. Thereafter, 21.2 g of 4-(2-(trans-4-propylcyclohexyl)ethyl)cyclohexanone (7) dissolved in 20 mL of THF was slowly added dropwise thereto at a temperature range of from 50 to 55° C., followed by stirring for 30 minutes. After cooling the resulting reaction mixture to 25° C., the reaction mixture was mixed with 100 mL of 3N hydrochloric acid and 100 mL of toluene in a vessel and separated into an organic layer and an aqueous layer by standing still, so as to attain extraction to the organic layer. The resulting organic layer was fractionated and washed with water, a 2N sodium hydroxide aqueous solution, a saturated sodium bicarbonate aqueous solution and water, followed by drying over anhydrous magnesium sulfate. Thereafter, the solvent was removed by distillation under reduced pressure to obtain 16.4 g of 1-(2-chloro-4-ethoxy-3-fluorophenyl)-4-(2-(trans-4-propylcyclohexyl)ethyl)cyclohexanol (8). The resulting compound (8) was a yellow solid matter.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2-chloro-4-ethoxy-3-fluorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Chisso Corporation; Chisso Petrochemical Corporation; US2008/75891; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 454-78-4,Some common heterocyclic compound, 454-78-4, name is 2-Bromo-1-chloro-4-(trifluoromethyl)benzene, molecular formula is C7H3BrClF3, 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-Bromo-4-chlorobenzotrifluoride and piperazine were dissolved in NMP (2 mL) and heated to 200C for 30 mins in a microwave reactor. NMP was removed using flash chromatography (1 :10 MeOH:DCM) to give 1-(2-bromo-4-(trifluoromethyl)phenyl) piperazine (RD71 ) which was used without further purification

The synthetic route of 454-78-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NATIONAL UNIVERSITY OF IRELAND, MAYNOOTH; STEPHENS, John; FINDLAY, John; KINSELLA, Gemma; MARTIN, Darren; DEVINE, Robert; VELASCO-TORRIJOS, Trinidad; WO2013/60860; (2013); A1;,
Chloride – Wikipedia,
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Reference of 320-50-3, The chemical industry reduces the impact on the environment during synthesis 320-50-3, name is 1,4-Dichloro-2-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

EXAMPLE 8 4-Chloro-2-trifluoromethylphenol To a 300 ml, 3-necked flask fitted with a stirrer, condenser, thermometer and drying tube is added dimethylsulfoxide (100 ml), tert-butanol (20 ml), powdered potassium hydroxide (KOH) pellets (85%, 30 g) and 2,5-dichlorobenzotrifluoride (21.5 g, 0.10 mole). The reaction mixture is warmed to 71-73 C. for 60 hours, then additional KOH (10 g) is added and heating is continued at 73-75 C. for 24 hours. The reaction mixture is cooled and the solvent partially removed by distillation at 0.9 mm, bp 55 C.). The cooled pot residue is then poured into ice water (1000 g) which had been preacidified to pH 1 with conc. HCl (50 ml). The aqueous mixture is extracted with carbon tetrachloride (CCl4), the CCl4 layer decanted and dried and the solvent removed under vacuum to afford 10.8 g of 4-chloro-2-trifluoromethylphenol, which is sublimed to afford pure product, mp 81-81.5 C. Elemental Anal. Calcd for C7 H4 ClF3 O: C, 42.75; H, 2.06; Cl, 18.04: Found: C, 42.54; H, 2.36; Cl, 18.16. STR14

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, 1,4-Dichloro-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Rohm and Haas Company; US4259510; (1981); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1009102-44-6,Some common heterocyclic compound, 1009102-44-6, name is 1-(4-Chlorophenyl)cyclopropanamine hydrochloride, molecular formula is C9H11Cl2N, 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:To a solution of methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)- 1 ,3,5-triazin-2- ylamino)benzoate (870 mg, 2.4 mmol) from Step 1 in THF (10 mL) was added l-(4- chlorophenyl)cyclopropanamine, HC1 (500 mg, 2,450 mmol) and Hunig’sBase (1.677 mL, 9.60 mmol). The resulting mixture was stiiTed for 16 h. The precipitate was filtrated through a plug washing with THF to give acrude product that was purified by Biotage eluting with 4/1-hexane/ethyl acetate to give 1.1 g of the desired product as a solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(4-Chlorophenyl)cyclopropanamine hydrochloride, its application will become more common.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; SUN, Li-Qiang; MULL, Eric; ZHAO, Qian; WANG, Tao; ZHANG, Zhongxing; SCOLA, Paul Michael; WO2012/24373; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 454-78-4, name is 2-Bromo-1-chloro-4-(trifluoromethyl)benzene, molecular formula is C7H3BrClF3, 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. Application In Synthesis of 2-Bromo-1-chloro-4-(trifluoromethyl)benzene

EXAMPLE 6; [5-(3-{4-[2-Chloro-5-(trifluoromethyl)phenyllpiperazin-l-yl|isoxazol-5-yl)-2//-tetrazol-2- yl] acetic acid; Step 1 : tert-Butyl 4-r2-chloro-5-(trifluoromethyl)phenyllpiperazine-l-carboxylate; Into a 50 mL pressure vial equipped with a magnetic stir bar was added tert-butyl piperazine-1-carboxylate (2.00 g, 10.7 mmol), palladium(II) acetate (0.24 g, 1.07 mmol) and racemic-BTNAP (1.34 g, 2.15 mmol). The vial was evacuated under vacuum (1 mm Hg) and backfilled with N2 (repeated 3 times). Toluene (10 mL) and 3-bromo-4-chlorobenzotrifluoride (3.06 g, 11.8 mmol) were added to the vial and the solvent was degassed for 10 min with a steady flow of nitrogen before being heated to 120 0C for 16 h. The reaction mixture was filtered through a plug of celite on a sintered glass funnel, washing with diethyl ether (100 mL). The filtrate was concentrated and purified by column chromatography through silica gel, eluting with 0% EtOAc in hexanes to 40% EtOAc in hexanes as a gradient. The desired product was obtained as a light yellow oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 454-78-4, its application will become more common.

Reference:
Patent; MERCK FROSST CANADA LTD.; ISABEL, Elise; LACHANCE, Nicolas; LECLERC, Jean-Philippe; LEGER, Serge; OBALLA, Renata, M.; POWELL, David; RAMTOHUL, Yeeman, K.; ROY, Patrick; TRANMER, Geoffrey, K.; ASPIOTIS, Renee; LI, Lianhai; MARTINS, Evelyn; WO2010/94126; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 1481-63-6, 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. 1481-63-6, name is 1-Bromo-2,4-dichloro-5-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 5 20 mmol of 2,4-dichloro-5-fluorobromobenzene, 180 mmol of phenylboronic acid, 240 mmol of potassium carbonate are heated with 0.1 mol % of trans-di-acetato-bis[o-(di-o-tolylphosphino)benzyl]dipalladium(II) in 300 ml of xylene for 16 hours at 130 C. The reaction solution is recrystallized after aqueous workup. Yield: 84% of 2,4-dichloro-5-fluorobiphenyl.

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-2,4-dichloro-5-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoechst AG; US5559277; (1996); A;,
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. 16429-44-0, name is 5-Bromo-3-chlorobenzene-1,2-diamine, A new synthetic method of this compound is introduced below., Recommanded Product: 16429-44-0

To a solution of 5-bromo-3-chlorobenzene-1,2-diamine (200 mg,0.90 mmol)inchloroform (3 mL)was added di(1H-imidazol-1-yl)methanone (220 mg,1.35 mmol). The mixture was heated to 60 C for 12 h under a nitrogen atmosphere. After cooling the reaction toroom temperature,the white precipitate was filtered off,washed with chloroform (3 mL x 2),and dried in vacuo to give the title compound (170 mg,76%)as a white solid. 1H NMR (400MHz,DMSO-d6)8 11.35 (s,1H),11.05 (s,1H),7.21 (d,J = 1.6 Hz,1H),7. 04 (d,J = 1.6 Hz,1H).

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; GENENTECH, INC.; CONSTELLATION PHARMACEUTICALS, INC.; CYR, Patrick; BRONNER, Sarah; ROMERO, F. Anthony; MAGNUSON, Steven; TSUI, Vickie Hsiao-Wei; WAI, John; LAI, Kwong Wah; WANG, Fei; (251 pag.)WO2017/205536; (2017); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics