HRID602158

反应详情

EQUATION

反应方程式

HRID 602158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

3-(tert-Butoxycarbonylamino)piperidine (7.07 g, 35.3 mmol) was dissolved in N,N-dimethylformamide (120 mL). To this solution, potassium carbonate (9.80 g, 70.9 mmol) and methyl 2-fluorobenzoate (5.0 mL, 39.2 mmol) were added and the mixture was stirred at 130° C. for 8 hours. Subsequently, the mixture was allowed to cool, diluted with ethyl acetate, and washed sequentially with water and brine. The washed product was dried over sodium sulfate and the solvent was evaporated. Purification of the resulting residue by silica gel column chromatography (hexane:ethyl acetate=10:1->5:1) gave 2.34 g (20%) of the desired compound as a yellow oil.

WORKUP

后处理

  1. temperatureto cool
  2. washwashed sequentially with water and brine
  3. dry with materialThe washed product was dried over sodium sulfate
  4. customthe solvent was evaporated
  5. customPurification of the resulting residue by silica gel column chromatography (hexane:ethyl acetate=10:1->5:1)