Month: May 2021

These common heterocyclic compound, 54773-19-2, name is 1,2-Dichloro-3-(trifluoromethyl)benzene, 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. COA of Formula: C7H3Cl2F3

EXAMPLE 5 Preparation of Compound No. 5 (Reaction (a)) A mixture of 1,2-dichloro-3-(trifluoromethyl)benzene (21.5 g), N-[(+-)-2-(4-hydroxyphenoxy)propionyl]isoxazolidine (23.7 g) which was prepared as in Example 3, anhydrous potassium carbonate (14.5 g) and dimethylsulfoxide (200 ml) was stirred at 130 C. for 3 hours. After the mixture was cooled, water and benzene were added thereto to form two layers. The organic layer thus separated was washed with 1 N aqueous sodium hydroxide solution and then with water and dried over anhydrous sodium sulfate. Removal of the solvent by a distillation in vacuo gave N-[(+-)-2-[4-(2-chloro-4-trifluoromethylphenoxy)phenoxy]propionyl]isoxazolidine (39.9 g) as a pale brown crystalline solid. Recrystallization from a mixture of n-hexane and ethyl acetate afforded a white crystalline solid. m.p. 66.5-67.5 C.

The synthetic route of 1,2-Dichloro-3-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hokko Chemical Industry Co., Ltd.; US4447259; (1984); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 56133-86-9, 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. 56133-86-9, name is 2-(2,5-Dichlorophenyl)ethanamine, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: Under nitrogen atmosphere, ethanol (30 mL), immediate III (3 mmol) and titanium (IV) isopropoxide (9 mmol) were added to a three-necked round bottom flask and stirred for 0.5 h, then the substituted ethylamine (3 mmol) was dropped into the solution and stirred for 3 h at room temperature. Subsequently, sodium borohydride (4.5 mmol) was added to the flask slowly, the reductive amination reaction was maintained for 3 h. According to the TLC monitoring results, the ammonia water (2 mol L-1, 10 mL) was poured into the flask to quench the reaction. The resulting mixture was filtered in vacuum and evaporated on rota vapor (Buchi). Hereafter, dissolved the residue with ethyl acetate (50 mL), and the solution was washed with 2 mol L-1 hydrochloric acid (30 mL), saturated aq NaHCO3 solution (30 mL), and brine (40 mL), successively, dried over anhydrous Na2SO4 and filtered. Solvent was evaporated in vacuum, and the residue was purified by silica gel column chromatography (petroleum ether / ethyl acetate as eluents). Finally, the samples were recrystallized from ethyl acetate / petroleum ether to afford target compounds with higher purity.

The chemical industry reduces the impact on the environment during synthesis 2-(2,5-Dichlorophenyl)ethanamine. I believe this compound will play a more active role in future production and life.

Reference:
Article; Cai, Nan; Cui, Zining; Feng, Zhihui; He, Lu; Ji, Mingshan; Li, Xinghai; Qi, Zhiqiu; Qin, Peiwen; Wang, Kai; Bioorganic and medicinal chemistry letters; (2019);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 7051-15-2, A common heterocyclic compound, 7051-15-2, name is 2-Chloro-1,3-dimethoxybenzene, molecular formula is C8H9ClO2, 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.

Example 1 3-Chloro-2,4-dimethoxybenzaldehyde (2a) was prepared from 1,3-dimethoxybenzene (1a) according to Plattner, J. J. et al. J. Med. Chem. 1984, 27 (8), 1016-1026. 3-(3-Chloro-2,4-dimethoxyphenyl)acrylic acid (3a).

The synthetic route of 7051-15-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Epoch Biosciences, Inc.; US2005/171340; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 451-85-4, A common heterocyclic compound, 451-85-4, name is 2,4-Dichloro-1-(trifluoromethoxy)benzene, molecular formula is C7H3Cl2F3O, 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.

Example 7 Trifluoromethoxybenzene was obtained at 230 C. from 2,4-dichloro-trifluoromethoxybenzene at a conversion of 100% and a selectivity of 91.4%.

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 Aktiengesellschaft; US5283378; (1994); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1000577-58-1,Some common heterocyclic compound, 1000577-58-1, name is 1-Bromo-2,3-dichloro-5-fluorobenzene, molecular formula is C6H2BrCl2F, 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.

l-Bromo-2,3-dichloro-5-fluorobenzene (1.0401 g, 4.27 mmol) was dissolved in toluene (30 mL), and then the solvent was removed under reduced pressure. The residue was dried under high vacuum for a few minutes. Anhydrous THF (15 mL) was added to dissolve the starting material. And then sodium methanoxide (0.9873 g, 17.36 mmol) was added. The mixture was heated at 75 C for 4.5 h, cooled to room temperature. The mixture was quenched with saturated ammonium chloride solution, concentrated to remove THF. The remaining mixture was extracted with ethyl acetate (4 x 150 mL). The organic solution was washed with brine, dried over anhydrous sodium sulfate, concentrated to dryness to afford 1.0188 g of product as white solid in 93% yield. -NMR (500MHz, CDC13): 7.109 (d, J = 3.0 Hz, 1H), 6.988 (d, J= 3.0 Hz, 1H), 3.786 (s, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,3-dichloro-5-fluorobenzene, its application will become more common.

Reference:
Patent; NEKTAR THERAPEUTICS (INDIA) PVT. LTD.; NEKTAR THERAPEUTICS; SHARMA, PANKAJ; KHATRI, VIJAY KUMAR; GU, XUYUAN; SONG, YUAN; SHEN, MICHAEL LIXIN; SAUTHIER, JENNIFER RIGGS; ANAND, NEEL K.; KOZLOWSKI, ANTONI; ODINECS, ALEKSANDRS; RILEY, TIMOTHY A.; REN, ZHONGXU; MU. YONGQI; SHEN, XIAOMING; YUAN. XUEJUN; AURRECOECHEA, NATALIA; O’MAHONY, DONOGH JOHN ROGER; WO2015/92819; (2015); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

127049-87-0, name is 1-Bromo-2,4-dichloro-3-methylbenzene, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Safety of 1-Bromo-2,4-dichloro-3-methylbenzene

To a stirred solution of 1-bromo-2,4-dichloro-3-methylbenzene (500 mg, 2.09 mmol) and 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (637 mg, 2.51 mmol) in 1.4- dioxane was added potassium acetate (304 mg, 3.10 mmol), and the mixture was degassed for 10 min. [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II) (Pd(dppf)Cl2; 152 mg, 0.2 mmol) was added, and the mixture was degassed for 10 min. The mixture was heated at 90 C for 5 h, was cooled and was diluted with EtOAc. The organic layer was washed with water and brine, dried over Na2S04, and concentrated. Purification by MPLC with 5% EtOAc- Hexane as eluent afforded the title compound as a colorless liquid (430 mg): *H NMR (300 MHz, CDCl3) delta 7.41 (dd, / = 2.07, 8.10 Hz, 1H), 7.26 – 7.23 (m, 1H), 2.47 (s, 3H), 1.37 (s, 12H). Note: The title compound obtained was impure (containing diborane) and used in next step without further purification.

The synthetic route of 127049-87-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DOW AGROSCIENCES LLC; BELL, Jared; BUYSSE, Ann M.; DAEUBLE, John F.; ECKELBARGER, Joseph D.; EPP, Jeffrey B.; IRVINE, Nicholas M.; KISTER, Jeremy; LO, William C.; LOSO, Michael R.; LOWE, Christian T.; ROHANNA, John C.; SATCHIVI, Norbert M.; SIDDALL, Thomas L.; STEWARD, Kimberly M.; YERKES, Carla N.; (281 pag.)WO2019/84353; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 621-62-5, name is 2-Chloro-1,1-diethoxyethane, 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 621-62-5, Application In Synthesis of 2-Chloro-1,1-diethoxyethane

A solution of 4-bromo-6-chloropyridazin-3-amine (15.7 g, 75.3 mmol), 2-chloro- 1,1- diethoxyethane (13.9 g, 90.3 mmol) and PTSA (17.2 g, 90.3 mmol) in isopropanol (150 mL) was heated to 80C for 20 h. After cooling to room temperature, the solution was concentrated in vacuo. The resulting mixture was treated with a saturated NaHC03 solution (300 mL), extracted with dichloromethane (200 mL x 3), dried over Na2S04, filtered and concentrated. The residue was purified by chromatography (silica gel, 200 – 300 mesh, petroleum ether : ethyl acetate = 3 : 1) to give 8-bromo-6-chloroimidazo[l,2-b]pyridazine (17.2 g, 98 %) as an orange solid. LC-MS: [M+H]+, 231.9, 233.9, tR = 1.46min

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HERMANN, Johannes Cornelius; KUGLSTATTER, Andreas; LUCAS, Matthew C.; PADILLA, Fernando; WANNER, Jutta; ZHANG, Xiaohu; WO2013/64445; (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. 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

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. 3260-88-6, name is 2-Methyl-3-chloroanisole, A new synthetic method of this compound is introduced below., Computed Properties of C8H9ClO

2-Chloro-6-methoxytoluene in an amount of 14.6 g (0.093 mole) was added with 100 ml methylene chloride and aluminium chloride in an amount of 24.9 g (0.187 mole), and acetyl chloride in an amount of 14.6 g (0.187 mole) was fed dropwise into the resulting mixture at 15 C. After stirring the mixture for an hour at an ambient temperature, the mixture was then poured into 1N-hydrochloric acid, and an organic layer obtained was washed with water and dried with anhydrous magnesium sulfate. The solvent remained in the layer was distillated out to obtain 2-chloro-4-methoxy-3-methylacetophenone in an amount of 18.1 g. The yield was 97.7%.

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; Nippon Soda Co., Ltd.; US6100421; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics