HRID1711096
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 a solution of the carboxylate 388 (1 g, 2.13 mmol) in DCM (4.3 mL) TFA (4.3 mL) was added and the reaction mixture was stirred 2 h at room temperature. The solvent was removed under reduced pressure, the residue was suspended in aqueous sodium bicarbonate, the mixture was extracted with DCM, EtOAc and DCM; the combined extracts were filtered and the recovered solids were collected and dried. The filtrate was dried over anhydrous Na2SO4, concentrated under reduced pressure and the residue was combined with the solid material obtained upon filtration, to afford 389 (806 mg, 100% yield) as a yellow solid. LCMS:(M+H) 372.1.
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- extractionthe mixture was extracted with DCM, EtOAc and DCM
- filtrationthe combined extracts were filtered
- customthe recovered solids were collected
- customdried
- dry with materialThe filtrate was dried over anhydrous Na2SO4
- concentrationconcentrated under reduced pressure
- customobtained upon filtration