HRID1265978

反应详情

EQUATION

反应方程式

HRID 1265978 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 50 ml flask equipped with a stirbar and septum and under an atmosphere of dry nitrogen was added 1.73 g (4.9 mmol) of 1-(α,α-dimethylbenzyl)-1-chloro-2,2-dibromocyclopropane and 12 ml of diethyl ether. After cooling in an ice bath for 10 minutes, 9.0 ml (12.6 mmol) of 1.4 M methyllithium in diethyl ether was added via syringe. A precipitate formed immediately. After stirring for 10 minutes the reaction was quenched with 3 ml of water. The aqueous layer was removed and the organic layer was dried over anhydrous magnesium sulfate and evaporated in vacuo with the bath temperature at +25° C. yielding 0.94 g of 1-(α,α-dimethylbenzyl)-cyclopropene.

WORKUP

后处理

  1. customInto a 50 ml flask equipped with a stirbar and septum and under an atmosphere of dry nitrogen
  2. temperatureAfter cooling in an ice bath for 10 minutes
  3. customA precipitate formed immediately
  4. customwas quenched with 3 ml of water
  5. customThe aqueous layer was removed
  6. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  7. customevaporated in vacuo with the bath temperature at +25° C.