反应详情

To half the material from step d (ca. 2.3 mmol) was added glyoxal (40% in water, 1 ml) and ethanol (15 ml) and the mixture heated to 100 deg C. After 1 hour the reaction was allowed to cool and was concentrated in vacuo. Water and dichloromethane was added and the mixture filtered under suction. The organic liquors were discarded and the aqueous layer was basified with 2N sodium hydroxide solution. To this was added dichloromethane and the mixture was again filtered under suction. The dichloromethane layer was separated and concentrated to furnish 289 mg of a yellow solid (80% clean). MS: [M+H]+198

1. temperaturethe mixture heated to 100 deg C
2. temperatureto cool
3. concentrationwas concentrated in vacuo
4. additionWater and dichloromethane was added
5. filtrationthe mixture filtered under suction
6. additionTo this was added dichloromethane
7. filtrationthe mixture was again filtered under suction
8. customThe dichloromethane layer was separated
9. concentrationconcentrated