HRID1809609

反应详情

EQUATION

反应方程式

HRID 1809609 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Tert-butyl 4-formylpiperidine-1-carboxylate (35.0 g, 164.1 mmol) was dissolved in dichloromethane (200 mL) and cooled to 0° C. Potassium tert-butoxide (23.9 g, 213 mmol) was added followed by addition of iodomethane (69.9 g, 492 mmol). The reaction was stirred at 0° C. for 30 minutes, and then warmed to ambient temperature and stirred for 1.5 hr. The reaction mixture was poured into brine (400 mL) and the organic layer was separated, dried, and filtered, and concentrated and purified by silica gel to provide tert-butyl 4-formyl-4-methylpiperidine-1-carboxylate (16.36 g, 72.0 mmol, 43.8% yield).

WORKUP

后处理

  1. temperaturewarmed to ambient temperature
  2. stirringstirred for 1.5 hr
  3. customthe organic layer was separated
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified by silica gel