HRID218457

反应详情

EQUATION

反应方程式

HRID 218457 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of cyano-2-piperidinylidene-ethanoic acid methyl ester (1.4 g, 7.76 mmol) in 25 mL 1M NaOH was heated at 100° C. for 30 mins. The reaction mixture was cooled to 0° C. and acidifed to pH 5-6 by adding conc. HCl, then extracted with 3×50 mL acetate. The organic phases were combined, dried, and concentrated. The crude product was purified on flash column to afford 2-piperidinylidene-ethanenitrile (590 mg, 62%).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. extractionextracted with 3×50 mL acetate
  3. customdried
  4. concentrationconcentrated
  5. customThe crude product was purified on flash column