HRID572478

反应详情

EQUATION

反应方程式

HRID 572478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A suspension of methyl 2-[(3S)-3,4-dihydroxy-1-butyn-1-yl]benzoate (500 mg, 2.270 mmol) in 1,2-Dichloroethane (DCE) (22 mL) was treated with dicyclohexylamine HBr (59.5 mg, 0.227 mmol) and then copper (II) bromide (1014 mg, 4.54 mmol) and stirred at 80° C. After 1.5 h, the reaction mixture was diluted with EtOAc, filtered through Celite and concentrated in vacuo. The residue was purified by silica gel chromatography (ethyl acetate-hexanes 0-70%) to afford the title compound (200 mg, 0.702 mmol, 31% yield) as brown solid: Rt=0.46 min,

WORKUP

后处理

  1. filtrationfiltered through Celite
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified by silica gel chromatography (ethyl acetate-hexanes 0-70%)