HRID2261099

反应详情

EQUATION

反应方程式

HRID 2261099 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,3-Dibromo-2,3-dihydro-benzo[1,4]oxazine-4,6-dicarboxylic acid 4-tert-butyl ester 6-methyl ester (767 mg, 1.7 mmol) from proceeding step was stirred in acetone (14 ml) at RT for 2 h with NaI (1.27 g, 8.5 mmol). The solvent was removed, EtOAc, water and 1 M sodium thiosulfate were added. After separating phases the organic layer was washed with brine. The solvent was concentrated and the crude was purified on silica gel using CH/EtOAc 7:3 to obtain a colorless oil (456 mg, 92%).

WORKUP

后处理

  1. customThe solvent was removed
  2. additionEtOAc, water and 1 M sodium thiosulfate were added
  3. customAfter separating phases the organic layer
  4. washwas washed with brine
  5. concentrationThe solvent was concentrated
  6. customthe crude was purified on silica gel using CH/EtOAc 7:3