HRID1838231

反应详情

EQUATION

反应方程式

HRID 1838231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 2.85 g portion of t-butyl 4-(4-cyano-3-trifluoromethylphenyl)-3-methylpiperazine-1-carboxylate synthesized in Reference Example 3 was stirred in 50 ml of trifluoroacetic acid at 0° C. to room temperature for 2 hours. The solvent was evaporated under reduced pressure, the resulting residue was neutralized with saturated aqueous sodium bicarbonate and then extracted with ethyl acetate, the organic layer was washed and dried and then the solvent was evaporated under reduced pressure. The residue was purified by a silica gel column chromatography, and 5.6 g of the title compound was obtained from chloroform-methanol-28% aqueous ammonia (10:1:0.1, v/v/v) eluate as light yellowish white crystals.

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washthe organic layer was washed
  4. customdried
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by a silica gel column chromatography