HRID428949

反应详情

EQUATION

反应方程式

HRID 428949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To tris(dibenzylideneacetone)dipalladiunm (0) (8.7 mg, 9.5 mmol) in tetrahydrofuran (2.5 ml) at room temperature was added triphenylarsine (12 mg, 39.2 [mol). After 10 min, a solution of 3-hexyl-6-(3-iodophenyl)-6-methyl-3-azabicyclo[3.1.0]hexan-2-one (Preparation 67, 0.15 g, 3.8 mmol) in tetrahydrofuran (2.5 ml) was added. A minute later, 4-(tributylstannyl)-1-triphenylmethyl-1H-imidazole (Preparation 73, 0.332 g, 0.55 mmol) in tetrahydrofuran (3 ml) was added. The reaction mixture was stirred at room temperature for 30 min and then refluxed for 3.5 h. The cooled reaction mixture was concentrated in vacuo and chromatographed on silica gel eluting with hexane:ethyl acetate (1:1 then 0:1) to give the title compound (55 mg, 25%).

WORKUP

后处理

  1. temperaturerefluxed for 3.5 h
  2. customThe cooled reaction mixture
  3. concentrationwas concentrated in vacuo
  4. customchromatographed on silica gel eluting with hexane:ethyl acetate (1:1