HRID1109431

反应详情

EQUATION

反应方程式

HRID 1109431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The reaction liquid was poured into water, and extracted with methylene chloride. The methylene chloride layer was washed with a diluted hydrochloric acid and water in this order. The organic layer thus recovered was distilled under a reduced pressure to remove the solvent, and subjected to purification by a silica gel chromatography (n-hexane:ethyl acetate=10:2) to obtain 1.9 g of p-nitrobenzoic acid 1,1,1-trifluoro-2-octyl ester. The ester was dissolved in 30 ml of ethanol, to which 0.19 g of 5% Pd-C catalyst was added. After the solution was stirred overnight under hydrogen atmosphere, the Pd-C catalyst was separated by filtration, and the ethanol was distilled off under a reduced pressure to obtain 1.8 g of p-aminobenzoic acid 1,1,1-trifluoro-2-octyl ester which was the desired compound of the reaction 1).

WORKUP

后处理

  1. additionwas added
  2. customthe Pd-C catalyst was separated by filtration
  3. distillationthe ethanol was distilled off under a reduced pressure