HRID262333

反应详情

EQUATION

反应方程式

HRID 262333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of n-butyllithium in hexane (224 ml; 2.2 M) was added to tetrahydrofuran (THF, 300 ml) at -60° followed by diiospropylamine (52 g) and this mixture was then warmed to room temperature stirred for 5 min and then cooled to -72° C. Methylisobutyrate (50 g) was then slowly added and the mixture was stirred for 11/2 hr at -70° C. Freshly distilled ethyl vinyl ketone (42 g) in THF (60 ml) was added to the above mixture over 10 min and the mixture was then stirred for a further 1/2 hr at -60° C. and subsequently at room temperature for 2 hr.

WORKUP

后处理

  1. temperaturecooled to -72° C
  2. stirringthe mixture was stirred for 11/2 hr at -70° C
  3. stirringthe mixture was then stirred for a further 1/2 hr at -60° C. and subsequently at room temperature for 2 hr