HRID914819

反应详情

EQUATION

反应方程式

HRID 914819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

After dissolving 230 mg of 2-methylphenol in 20 ml of N,N-dimethylformamide, 43 mg of sodium hydride (70% suspension in oil) was added and the mixture was stirred at 80° C. for 30 minutes. Next, 224 mg of 1-(tert-butoxycarbonyl)-4-cyano-4-(methanesulfonyloxymethyl)piperidine was added and the mixture was stirred at 100° C. for 8 hours. After cooling it to room temperature, water was added and extraction was performed with ethyl acetate. The organic layer was washed with a 1N sodium hydroxide solution and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (273 mg, 100% yield).

WORKUP

后处理

  1. additionwas added
  2. stirringthe mixture was stirred at 100° C. for 8 hours
  3. temperatureAfter cooling it to room temperature
  4. extractionextraction
  5. washThe organic layer was washed with a 1N sodium hydroxide solution
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure