4-chloro-1-methyl-2-(trifluoromethyl)benzene

Conditions: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 1000-ml autoclave which is equipped with a mechanical stirrer and made of stainless steel (SUS-316) was charged with 263.6 g (1.0 mol) of the isomeric mixture (the product of the first step) containing 0.72 mol of 2-trifluoromethyl-4-chlorobenzalchloride as a main component, 84 g (2.1 mol) of sodium hydroxide and 420 g of water. Then, 5.3 g (2.0 wt %) of a metal-carried catalyst (5%-Pd/carbon) was added to the autoclave. The atmosphere of the autoclave was replaced by hydrogen, and the autoclave was put into oil bath to increase the temperature to 30° C. At the same time, stir was started while the hydrogen pressure was maintained at 5 kg/cm2. This started absorption of hydrogen. After the lapse of 4 hr, stir was stopped, and the reaction liquid was allowed to cool down. By analysis, conversion of 2-trifluoromethyl-4-chlorobenzalchloride (purity: 72.1%) was 99.9%. Then, the catalyst and the salt were removed by vacuum filtration. The resultant solution was put into a 1000-ml separating funnel, and then the aqueous phase was removed. The organic phase was washed with 500 ml of water and dried with magnesium sulfate. Then, magnesium sulfate was removed by vacuum filtration. As the result, 171.6 g of 2-methyl-5-chlorobenzotrifluoride (purity: 63.8%) was obtained. The yield of this product was 79.0%. A 1000-ml autoclave which is equipped with a mechanical stirrer the autoclave was put into oil bath was maintained at 5 kg/cm2 This started absorption of hydrogen After the lapse of 4 hr, stir the reaction liquid to cool down Then, the catalyst and the salt were removed by vacuum filtration separating funnel the aqueous phase was removed The organic phase was washed with 500 ml of water dried with magnesium sulfate Then, magnesium sulfate was removed by vacuum filtration

Conditions: temp:30.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A 1000-ml autoclave which is equipped with a mechanical stirrer and made of stainless steel (SUS-316) was charged with 263.6 g (1.0 mol) of the isomeric mixture (the product of the first step) containing 0.72 mol of 2-trifluoromethyl-4-chlorobenzalchloride as a main component, 84 g (2.1 mol) of sodium hydroxide and 420 g of water. Then, 5.3 g (2.0 wt %) of a metal-carried catalyst (5%-Pd/carbon) was added to the autoclave. The atmosphere of the autoclave was replaced by hydrogen, and the autoclave was put into oil bath to increase the temperature to 30° C. At the same time, stir was started while the hydrogen pressure was maintained at 5 kg/cm2. This started absorption of hydrogen. After the lapse of 4 hr, stir was stopped, and the reaction liquid was allowed to cool down. By analysis, conversion of 2-trifluoromethyl-4-chlorobenzalchloride (purity: 72.1%) was 99.9%. Then, the catalyst and the salt were removed by vacuum filtration. The resultant solution was put into a 1000-ml separating funnel, and then the aqueous phase was removed. The organic phase was washed with 500 ml of water and dried with magnesium sulfate. Then, magnesium sulfate was removed by vacuum filtration. As the result, 171.6 g of 2-methyl-5-chlorobenzotrifluoride (purity: 63.8%) was obtained. The yield of this product was 79.0%. A 1000-ml autoclave which is equipped with a mechanical stirrer the autoclave was put into oil bath was maintained at 5 kg/cm2 This started absorption of hydrogen After the lapse of 4 hr, stir the reaction liquid to cool down Then, the catalyst and the salt were removed by vacuum filtration separating funnel the aqueous phase was removed The organic phase was washed with 500 ml of water dried with magnesium sulfate Then, magnesium sulfate was removed by vacuum filtration

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 2-Trifluoromethyl-4-chloro-benzalchloride and 2-methyl-3-nitro-5-chlorobenzotrifluoride, are intermediates in a process of preparing 2-methyl-3-aminobenzo-trifluoride. In this process, 2-trifluoromethyl-4-chlorobenzal-chloride is prepared by chlorinating o-trifluoromethylbenzalhalide, and 2-methyl-3-nitro-5-chlorobenzotrifluoride is prepared at first by hydrogenating the 2-trifluoro-methyl-4-chlorobenzalhalide to form a 2-methyl-5-monochlorobenzotrifluoride and then by nitrating the 2-methyl-5-monochlorobenzotrifluoride. Following this process, 2-methyl-3-aminobenzotrifluoride (MA-BTF) is prepared by hydrogenating the 2-methyl-3-nitro-5-chlorobenzotrifluoride. The thus prepared 2-methyl-3-aminobenzotrifluoride is useful as an intermediate in preparing medicines, agricultural chemicals and other chemical products. is prepared at first