HRID2165503

反应详情

EQUATION

反应方程式

HRID 2165503 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

15.4 g (0.093 mol) of 3-methyl-3,4,5,6-tetrahydrophthalic acid anhydride are dissolved in 90 ml of toluene. 18.4 g (0.093 mol) of 4-chloro-2-fluoro-5-isopropoxyaniline and 0.6 g of dimethylaminopyridine are added and the mixture is heated until the solvent and the water that has formed distil off. After approximately 2 hours at a bath temperature of 145° C. the reaction is complete. The residue is chromatographed over a column of silica gel with hexane/ethyl acetate 9:1. As main fraction there are obtained 26.8 g (82.0%) of the title compound (Compound No. 1.030) of the formula ##STR9## in the form of an oil, nD22 =1.5458.

WORKUP

后处理

  1. temperaturethe mixture is heated until the solvent
  2. customdistil off
  3. customThe residue is chromatographed over a column of silica gel with hexane/ethyl acetate 9:1