HRID751130
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
To intermediate 61C (0.1 M solution in 10% CH3CN in DCM) add NMO (2 equiv) followed by TPAP (0.05 equiv). Provide sufficient ventilation and take care to watch for exotherm. Stir reaction at rt for 3-5 h. Dilute by half with hexane and allow TPAP to precipitate. Flash filter through silica gel plug (20 fold mass of starting alcohol) and elute with 10% EtOAc/Hex until product is not observed in eluent. Removal of solvents gave the title compound. MS (ES) m/z 344.31 [M+H]+
WORKUP
后处理
- customProvide sufficient ventilation
- customreaction at rt for 3-5 h
- customto precipitate
- filtrationFlash filter through silica gel plug (20 fold mass of starting alcohol)
- washelute with 10% EtOAc/Hex until product
- customRemoval of solvents