HRID2257492

反应详情

EQUATION

反应方程式

HRID 2257492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Magnesium (3.0 g) was stirred in methanol, carbon tetrachloride (0.5 ml) added and the mixture waged at 50° C. until the metal had dissolved (1.5 hours). Tert-butyl 3-cyclopropyl-3-oxopropanoate (20.0 g) was then added dropwise and the mixture heated under reflux conditions for 1 hour. The solvent was evaporated and re-evaporated after addition of toluene to give tert-butyl 3-cyclopropyl-3-oxopropanoate magnesium salt (29.9 g) as a white solid, m.p. >300° C., IR max (C=O) 1520, 1540; (C-O) 1350 cm-1.

WORKUP

后处理

  1. customwaged at 50° C. until the metal
  2. dissolutionhad dissolved (1.5 hours)
  3. temperaturethe mixture heated under reflux conditions for 1 hour
  4. customThe solvent was evaporated
  5. customre-evaporated
  6. additionafter addition of toluene