反应详情

Citric acid monohydrate (10.39 g, 49.46 mmol) was added to a solution of 3-(benzhydrylidene-amino)-1-methyl-3-prop-2-ynyl-pyrrolidin-2-one (6.26 g, 19.79 mmol) (which may be prepared as described in Description 2) in THF (150 mL) and the reaction was stirred at room temperature for 18 hours. A colourless solid precipitated out. The solvent was evaporated to give a gummy white solid. This was trituated with Et2O and the solid was washed with further Et2O. The solid was suspended in water/MeOH and purified by SCX (70 g Silca), eluting with water/MeOH, MeOH and finally 0.5M NH3 in MeOH. Fractions containing product were evaporated to afford 3-amino-1-methyl-3-prop-2-ynyl-pyrrolidin-2-one (3.23 g, 21.223 mmol) as a pale yellow oil;

1. customA colourless solid precipitated out
2. customThe solvent was evaporated
3. customto give a gummy white solid
4. washthe solid was washed with further Et2O
5. custompurified by SCX (70 g Silca)
6. washeluting with water/MeOH, MeOH and finally 0.5M NH3 in MeOH
7. additionFractions containing product
8. customwere evaporated