反应 #1478439
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05968408
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: The reaction sequence set out in FIG. 4 is as follows: 3-chloro-2-methylacetanilide was prepared from 3-chloro-2-methylaniline via acetylation of the aniline with acetic anhydride in an aqueous methanol solution. A mixture of chloro-methylnitro-acetanilide isomers was thereafter formed by nitration of the acetanilide with sulfuric and nitric acid. The 3-chloro-2-methyl4-nitro isomer was removed by precipitation after addition of potassium hydroxide to the mixture of isomer in ethanol. The 3-chloro-2-methyl-6-nitroacetanilide was heated to reflux in an aqueous sodium hydroxide solution. The solid that formed was 3-chloro-2-methyl-6-nitroaniline. Reaction with a solution of stannous chloride in hydrochloric acid yielded a precipitate of 4-chloro-3-methyl-1,2-benzenediamine. Reaction with sodium nitrite in acetic acid yielded a solid 5-chloro4-methylbenzotriazole. The 3-chloro-2-methyl4-nitro isomer was removed by precipitation after addition of potassium hydroxide to the mixture of isomer in ethanol The 3-chloro-2-methyl-6-nitroacetanilide was heated to reflux in an aqueous sodium hydroxide solution The solid that formed
来源 ID: ord-64d333f6281443a89f3330f54caff650