HRID660575
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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
To a solution of methanesulfonic acid 7-oxo-6,7-dihydro-5H-dibenzo[c,e]azepin-5-ylmethyl ester in acetone (5 mL) is added NaI and the mixture is stirred at 50° C. for 18 h. The solvent is removed under reduced pressure and EtOAc is added. The solution is washed sequentially with sodium bisulfite solution, water and brine and is dried over magnesium sulfate. The solvent is removed under reduced pressure and the residue purified by flash chromatography using a gradient of 0-100% EtOAc/hexane as eluent to give the title compound as a yellow solid.
WORKUP
后处理
- customThe solvent is removed under reduced pressure and EtOAc
- additionis added
- washThe solution is washed sequentially with sodium bisulfite solution, water and brine
- dry with materialis dried over magnesium sulfate
- customThe solvent is removed under reduced pressure
- customthe residue purified by flash chromatography