HRID459798

反应详情

EQUATION

反应方程式

HRID 459798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (2-Amino-6-bromo-phenyl)-methanol (549 mg, 2.72 mmol) and triphosgen (282 mg, 0.95 mmol) in THF (20 ml) was heated at 50° C. for an hours. After cooling to room temperature, the reaction mixture was partitioned between water and ethyl acetate. The organic layer was washed by water and brine. After drying over MgSO4, the solution was concentrated under vacuum to give 5-bromo-1,4-dihydro-benzo[d][1,3]oxazin-2-one (582 mg, 94%) as a white solid. MS: 226.1 (M−H)−. (M+H)−.

WORKUP

后处理

  1. customthe reaction mixture was partitioned between water and ethyl acetate
  2. washThe organic layer was washed by water and brine
  3. dry with materialAfter drying over MgSO4
  4. concentrationthe solution was concentrated under vacuum