HRID2186449

反应详情

EQUATION

反应方程式

HRID 2186449 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of boron tribromide (25.6 ml of a 1.0M in dichloromethane) was added slowly to a stirred solution of 7-bromo-4-methoxy-2-(morpholin-4-yl)-benzooxazole (4.0 g) in dry dichloromethane (100 ml) under an atmosphere of nitrogen. The reaction mixture was stirred at room temperature for 90 mins. The mixture was partitioned between sodium hydrogencarbonate solution (50 ml) and dichloromethane (100 ml). The organic layer was separated, dried over magnesium sulphate, filtered and the solvent removed in vacuo. Purification by column chromatography on silica eluting with 30-50% ethyl acetate in heptane afforded the title compound as an off-white solid (1.64 g).

WORKUP

后处理

  1. customThe mixture was partitioned between sodium hydrogencarbonate solution (50 ml) and dichloromethane (100 ml)
  2. customThe organic layer was separated
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customthe solvent removed in vacuo
  6. customPurification by column chromatography on silica eluting with 30-50% ethyl acetate in heptane