HRID892612

反应详情

EQUATION

反应方程式

HRID 892612 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. additionwas added
  2. temperatureunder ice-cooling
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with a saturated aqueous solution of sodium bicarbonate and saturated brine in sequence
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. concentrationfollowed by concentration
  7. customThe residue was purified by PLC (chloroform:methanol=49:1)