HRID1838230

反应详情

EQUATION

反应方程式

HRID 1838230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 4.46 g portion of t-butyl 3-methylpiperazine-1-carboxylate synthesized in Reference Example 2, 6.74 g of 4-fluoro-2-trifluoromethylbenzonitrile and 7.76 ml of diisopropylethylamine were stirred in 50 ml of DMF at 100° C. for 2 days. The reaction solution was diluted with water and extracted with ethyl acetate, the organic layer was washed and dried and then the solvent was evaporated under reduced pressure. The residue was subjected to a silica gel column chromatography and eluted with hexane-ethyl acetate (3:1, v/v) to obtain 5.6 g of the title compound as white crystals.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washthe organic layer was washed
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. washeluted with hexane-ethyl acetate (3:1