HRID2170859

反应详情

EQUATION

反应方程式

HRID 2170859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a stirred solution of 4-(4-chlorophenoxy)piperidine hydrochloride (300 mg, 1.21 mmol), 1H-indole-5-carboxylic acid (195 mg, 1.21 mmol), and N,N-diisopropylethylamine (0.85 mL, 4.84 mmol) in N,N-dimethylformamide (10 mL) was add HBTU (688 mg, 1.81 mmol) at room temperature. After stirring at 60° C. for 2 hours, the mixture was poured into water (50 mL). This was extracted with ethyl acetate (50 mL) and washed with water (50 mL). The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica-gel column chromatography (NH-gel, eluting with n-hexane/ethyl acetate=1/1) to give 403 mg (94% yield) of the title compound as a white solid.

WORKUP

后处理

  1. extractionThis was extracted with ethyl acetate (50 mL)
  2. washwashed with water (50 mL)
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica-gel column chromatography (NH-gel, eluting with n-hexane/ethyl acetate=1/1)