HRID1765357

反应详情

EQUATION

反应方程式

HRID 1765357 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 4-Bromo-7-hydroxymethyl-2-isopropyl-2H-phthalazin-1-one (0.74 g, 2.5 mmol) in acetonitrile (5 ml) was added dropwise to a stirred suspension of trimethylsilyl bromide (TMSBr) (0.9 g, 6.3 mmol) and LiBr (0.41 g, 5 mmol) in acetonitrile (15 ml). The reaction mixture was heated to 80° C. for 24 hours, after which time the reaction mixture was cooled to room temperature and the solvent removed under vacuum. The resulting residue was purified by flash column chromatography (elution: 85% heptane, 15% ethyl acetate) to give the title compound (0.4 g, 44% yield) as a white solid.

WORKUP

后处理

  1. temperatureafter which time the reaction mixture was cooled to room temperature
  2. customthe solvent removed under vacuum
  3. customThe resulting residue was purified by flash column chromatography (elution: 85% heptane, 15% ethyl acetate)