HRID261456

反应详情

EQUATION

反应方程式

HRID 261456 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 13.0 g (0.050 mol) of methyl 2,2-dimethyl-3-(2,2,2-trichloroethyl)cyclopropane-1-carboxylate (compound Z, C/T=77/23), 9.12 g (0.060 mol) of 1,5-diazabicyclo[5.4.0]undec-5-ene and 50 ml of dimethylformamide was stirred at 100° for 1 hour, then allowed to cool to room temperature and poured into 1 N hydrochloric acid. The mixture was extracted with ether and the ether extracts were combined, washed with brine, dried over magnesium sulfate and concentrated to give 10.15 g (91% yield) of methyl 3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylate, 94% purity, C/T=76/24.

WORKUP

后处理

  1. extractionThe mixture was extracted with ether
  2. washwashed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated