Month: May 2021

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. 69411-05-8, name is 3-Chloro-5-trifluoromethylaniline, This compound has unique chemical properties. The synthetic route is as follows., name: 3-Chloro-5-trifluoromethylaniline

To a mixture of 3-chloro-5-(trifluoromethyl)aniline (3.25 g, 16.6 mmol, Eq: 1.00) in dimethylsulfoxide (43.4 ml) was added N-bromosuccinimide (3.11 g, 17.4 mmol, Eq: 1.05) in 5 portions over 2.5 hr (622 mg each 30 min). 2h after the last addition, the reaction mixture was partitioned between 10% aqueous sodium sulfite and ethyl acetate. The organic layer was washed with aqueous sat. sodium carbonate, water (3 times) and brine then adsorbed unto silica (6g) and purified on silica gel (column 120 g, Hexane/ethyl acetate 90: 10 to 65:35) to give 4.36 g (96%) of a yellow solid. MS +m/z: 275.8 (M+H)+

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 69411-05-8.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; PLANCHER, Jean-Marc; WEIKERT, Robert James; WO2014/135423; (2014); 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. 6626-57-9, name is 1,3-Dichloro-2,2-dimethoxypropane, A new synthetic method of this compound is introduced below., Product Details of 6626-57-9

The last step was dissolved in 125mL solid 42.24g methylene chloride: water = 6: 1 in a mixed solvent, at 20-35 under fed 42.0g chlorine, chlorine was stopped and stirring was continued for 0.5 hours, after standing points the aqueous layer, the organic layer was dried over anhydrous magnesium sulfate, and the solvent evaporated under reduced pressure and the low-boiling by-products, 1,3-dichloro-acetone to give a colorless liquid 30.45 g, 97.7% pure by gas chromatography, a yield of 96.2%

The synthetic route of 6626-57-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Southeast University; Wang, MingLiang; Wang, Jia; Dan, hongbin; Gu, xiantao; Wang, shengzhi; Zhang, Wei; (5 pag.)CN105461529; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 69411-05-8, A common heterocyclic compound, 69411-05-8, name is 3-Chloro-5-trifluoromethylaniline, molecular formula is C7H5ClF3N, 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: To a solution of 3-chloroaniline 5a (37mg, 0.33mmol) in H2O (10mL cooled to-5C) was added 0.2mL of 2N HCl (aq.). To the resulting acidic aniline solution, 1N solution of sodium nitrite (0.33mL, 0.33mmol) was added dropwise to generate the aryldiazonium salt solution 6a. To the aryldiazonium salt solution was added sodium acetate (54mg, 0.66mmol), followed by 1mL solution of crude 3-oxo-3-(3-phenylisoxazol-5-yl)propanenitrile 4a (88mg, 0.33mmol) in ethanol. The reaction mixture was stirred at 0C for 5min, and then poured onto H2O (10mL) and extracted with ethyl acetate (20mL). The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by short column chromatography on silica gel, eluting with hexane/ethyl acetate (2/1) to provide the desired product 7 (67mg, 50% for two steps from 3a) as a yellow solid.

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:
Article; Ye, Na; Zhu, Yingmin; Liu, Zhiqing; Mei, Fang C.; Chen, Haiying; Wang, Pingyuan; Cheng, Xiaodong; Zhou, Jia; European Journal of Medicinal Chemistry; vol. 134; (2017); p. 62 – 71;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 120758-03-4,Some common heterocyclic compound, 120758-03-4, name is 2-Chloro-3,5-dimethoxyaniline, molecular formula is C8H10ClNO2, 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.

A mixture of 1-(2,4,6-trifluorophenyl)-1-propanone (7.0 g, 37.2 mmol), 2-chloro-3,5-dimethoxybenzenamine (see European Patent 1333028 for a method of preparation) (6.96 g, 37.1 mmol) and p-toluenesulfonic acid (1.41 g, 8.2 mmol) in toluene (80 mL) was heated at reflux with use of a Dean-Stark trap to remove water. After 20 h, the reaction mixture was cooled to room temperature and diluted with ethyl acetate. The organic layer was washed with water, sulfuric acid (1 N), water and saturated aqueous sodium chloride solution. The organic layer was dried (Na2SO4), filtered and concentrated to provide the title compound (10 g) which was used without further purification in Step C below.

The synthetic route of 120758-03-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E.I. DU PONT DE NEMOURS AND COMPANY; US2010/160385; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 69411-05-8, 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.

General procedure: To a solution of 3-chloroaniline 5a (37mg, 0.33mmol) in H2O (10mL cooled to-5C) was added 0.2mL of 2N HCl (aq.). To the resulting acidic aniline solution, 1N solution of sodium nitrite (0.33mL, 0.33mmol) was added dropwise to generate the aryldiazonium salt solution 6a. To the aryldiazonium salt solution was added sodium acetate (54mg, 0.66mmol), followed by 1mL solution of crude 3-oxo-3-(3-phenylisoxazol-5-yl)propanenitrile 4a (88mg, 0.33mmol) in ethanol. The reaction mixture was stirred at 0C for 5min, and then poured onto H2O (10mL) and extracted with ethyl acetate (20mL). The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by short column chromatography on silica gel, eluting with hexane/ethyl acetate (2/1) to provide the desired product 7 (67mg, 50% for two steps from 3a) as a yellow solid.

The synthetic route of 3-Chloro-5-trifluoromethylaniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ye, Na; Zhu, Yingmin; Liu, Zhiqing; Mei, Fang C.; Chen, Haiying; Wang, Pingyuan; Cheng, Xiaodong; Zhou, Jia; European Journal of Medicinal Chemistry; vol. 134; (2017); p. 62 – 71;,
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. 179897-90-6, name is 1,3-Dibromo-2-chloro-5-fluorobenzene, A new synthetic method of this compound is introduced below., COA of Formula: C6H2Br2ClF

EXAMPLE 185 6-(3-Bromo-2-chloro-5-fluorophenyl)-1,2-dihydro-2,2,4-trimethylquinoline (Compound 285, Structure 4 of Scheme II, where R1 =3-bromo-2-chloro-5-fluorophenyl) This compound was prepared according to General Method 2 (EXAMPLE 9) from Compound 9 (143.3 mg, 0.45 mmol) and 1-chloro-2,6-dibromo-4-fluorobenzene (129.9 mg, 0.45 mmol). The crude material was purified by flash column chromatography (50 mL silica, hexane) followed by reverse phase preparatory TLC (1000 mL ODS, 80% methanol/water) to afford 4.3 mg (3%) of Compound 285. Data for Compound 285: 1 H NMR (400 MHz, acetone-d6) 7.50 (dd, J=7.8, 3.0, 1 H), 7.19 (dd, J=9.2, 3.0, 1 H), 7.10 (d, J=2.0, 1 H), 7.03 (dd, J=8.1, 2.0, 1 H), 6.55 (d, J=8.3, 1 H), 5.61 (s, 1 H), 5.37 (s, 1 H), 1.97 (s, 3 H), 1.29 (s, 6 H).

The synthetic route of 179897-90-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ligand Pharmaceuticals Incorporated; US5693646; (1997); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1481-63-6, name is 1-Bromo-2,4-dichloro-5-fluorobenzene, 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 1481-63-6, COA of Formula: C6H2BrCl2F

EXAMPLE In a 500 ml three-necked flask equipped with reflux condenser and vane stirrer, 243.89 g (1 mol) of 5-bromo-2,4-dichlorofluorobenzene, 80.61 g (0.9 mol) of copper(I) cyanide and 70 g (0.81 mol) of dimethylacetamide are initially introduced into the reaction vessel and heated to 150 C. The reaction suspension is maintained for a further 4 to 5 hours at this temperature with vigorous stirring. Subsequently, it is cooled to 40 C. to 50 C. and the precipitated salts are filtered off by suction. The filter cake is washed 3 times each with 50 ml of methylene chloride and the combined organic phases are fractionally distilled together with the mother liquor. In addition to 39.0 g of 5-bromo-2,4-dichlorofluorobenzene, 127.6 g (80.1%) of 2,4-dichloro-5-fluorobenzonitrile are obtained, relative to reacted 5-bromo-2,4-dichlorofluorobenzene, having a purity (GC) >98%.

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; Hoechst Aktiengesellschaft; US5187295; (1993); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 204930-37-0, 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. 204930-37-0, name is 5-Bromo-1,3-dichloro-2-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

Preparation 3; 5-bromo-2-(bromomethyl)- 1 ,3-dichlorobenzene; Heat a solution of 5-bromo-l,3-dichloro-2-methylbenzene (97 mg, 0.40 mmol),N-bromosuccinimide (76 mg, 0.425 mmol) and benzoyl peroxide (16 mg, 0.06 mmol) in CCl4 (5 mL) to reflux for 3 hours under N2. Cool the reaction to room temperature and concentrate to an orange residue. Purify the residue by silica gel chromatography eluting with hexanes to afford 112 mg (87percent) of the product as white crystals.

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

Reference:
Patent; ELI LILLY AND COMPANY; WO2007/127763; (2007); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 928-50-7, 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. 928-50-7, name is 5-Chloropent-1-ene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: With the dissolution of substrate (0.4 mmol) in CH 3 CN (2 mL), Pd0/RGO (0.01 g), H 2 O (0.5 mL), and GO (0.01 g) were orderly added into apressure bottle (35 mL). The mixture was dispersed by ultrasound forabout 30 min at 25 C. Then H 2 O 2 (30 wt%, 4 mmol) was cautiously added dropwise. Immediately, the reaction system was heated to 55 Cwith lid closed until the process was fully completed (detected by TLC).Subsequently, Pd0/RGO and GO were removed by centrifuge. Themixture was extracted by deionized water and ethyl acetate. After thelayers were separated, the organic part was washed with deionizedwater, dried with anhydrous NaSO 4 , ltered and evaporated by reducedpressure distillation. Finally, purication of the crude product wascarried out by column chromatography. For 14, 18, 24, 40 (Table 2),excess hydrogen peroxide was added after half of the total reaction time.

The synthetic route of 5-Chloropent-1-ene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gao, Xi; Zhou, Jianhao; Peng, Xinhua; Catalysis Communications; vol. 122; (2019); p. 73 – 78;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 5211-02-9, These common heterocyclic compound, 5211-02-9, name is 3-Chloro-4-ethoxyaniline, 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.

4-Bromo-7-fluoro-1H-indole-2-carboxylic acid ethyl ester (200 mg, 0.7 mmol) was dissolved in toluene (16 mL), and Pd2 (dba) 3 (64 mg, 0.07 mmol) and Davephos (55 mg) were sequentially added. , 0.14 mmol) and K3PO4 (446 mg, 2.1 mmol, 2.1 mL of H2O), and after stirring well, 2- (4-amino-2-chlorophenoxy) ethyl-1-yl (394 mg, 2.10 mmol) of toluene ( 4mL) solution, under the protection of argon, refluxed for 20h. Cool to room temperature, concentrate, add EA (30mL) to dissolve the residue, 5N hydrochloric acid (20mL), saturated brine (20mL ¡Á 3), extract with water (20mL ¡Á 2), dry over anhydrous magnesium sulfate, and column chromatography (P / E = 5: 1 to 3: 1) 82 mg of a yellow solid was obtained with a yield of 29.9% and melting point: 191-192 C.

The synthetic route of 5211-02-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Medical Sciences Pharmaceutical Institute; Xu Boling; Chen Xiaoguang; Cui Guonan; Lai Fangfang; Zhou Jie; Ji Ming; Wang Xiaoyu; Du Tingting; Li Ling; Jin Jing; (144 pag.)CN110483366; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics