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
N-[(4-Oxo-4-(2-oxo-1-pyrrolidinyl)butanoyl]-L-prolinol (105 mg) was dissolved in a mixed solvent of benzene (0.25 ml), DMSO (0.79 ml) and triethylamine (0.25 ml), and sulfur trioxide pyridine complex (285 mg) was added thereto under ice-cooling. After 0.5 hour's stirring at a temperature of 10°-15° C., the reaction mixture was poured into ice water, and extracted with chloroform. The organic layer was washed with a saturated aqueous solution of sodium bicarbonate and saturated brine in sequence. The organic layer was dried over magnesium sulfate, followed by concentration. The residue was purified by PLC (chloroform:methanol=49:1) using silica gel to give 65 mg of N-[(4-oxo-4-(2-oxo-pyrrolidinyl)butanoyl]-L-prolinal.
WORKUP
后处理
- additionwas added
- temperatureunder ice-cooling
- extractionextracted with chloroform
- washThe organic layer was washed with a saturated aqueous solution of sodium bicarbonate and saturated brine in sequence
- dry with materialThe organic layer was dried over magnesium sulfate
- concentrationfollowed by concentration
- customThe residue was purified by PLC (chloroform:methanol=49:1)