HRID2261099
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was removed
- additionEtOAc, water and 1 M sodium thiosulfate were added
- customAfter separating phases the organic layer
- washwas washed with brine
- concentrationThe solvent was concentrated
- customthe crude was purified on silica gel using CH/EtOAc 7:3