HRID1180377

反应详情

EQUATION

反应方程式

HRID 1180377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the crude compound of 4-[hydroxy(phenyl)methyl]benzoic acid (1.51 g, 6.6 mmol) in DMF (33 mL) was added tert-butyl piperazine-1-carboxylate (1.23 g, 6.6 mmol), triethylamine (3.7 mL, 26.5 mmol) and HATU (2.51 g, 6.6 mmol). The mixture was aged for 3 hours under a nitrogen atmosphere and was then poured into a saturated aqueous solution of NaHCO3. The resulting mixture was extracted 3 times with ethyl acetate. The combined organic layers were washed with brine, dried and evaporated to a solid which was stirred in ethyl acetate at room temperature for 2 hours. The title compound was then recovered by filtration as a white solid.

WORKUP

后处理

  1. extractionThe resulting mixture was extracted 3 times with ethyl acetate
  2. washThe combined organic layers were washed with brine
  3. customdried
  4. customevaporated to a solid which
  5. filtrationThe title compound was then recovered by filtration as a white solid