反应详情

To a solution of N-carbethoxy-4-piperidone (11.34 g, 66.24 mmol) in nitromethane (5.3 mL) and ethanol (2 mL) was added a solution of sodium ethoxide in ethanol (2.67 M, 1.24 mL, 3.31 mmol). The mixture was stirred for 5 min and a solution formed from which a solid precipitated. After 1.5 h, water (100 mL) was added and the solid was isolated by filtration, washed with water (100 mL), and dried under vacuum with heat to yield the product ethyl 4-hydroxy-4-(nitromethyl)piperidine-1-carboxylate as an off white solid, 9.58 g (62%).

1. customa solution formed from which a solid
2. customprecipitated
3. waitAfter 1.5 h
4. additionwater (100 mL) was added
5. customthe solid was isolated by filtration
6. washwashed with water (100 mL)
7. customdried under vacuum
8. temperaturewith heat