反应详情

温度

80 °C

A stirred mixture of 5-amino-4-oxopentanoic acid hydrobromide (1.60 g, 7.5 mmol), benzyl alcohol (15 ml), and 48% hydrobromic acid (8 drops) was heated to 80° C. (bath temperature) for 2 days. The mixture was cooled to room temperature and excess benzyl alcohol was removed with a rotary evaporator at 0.12 mm Hg. The residue was titrated with diethyl ether (2×50 ml) and the residue was purified by flash chromatography on a 160×55 mm silica gel 60 column eluted sequentially with acetonitrile, 50 methanol in acetonitrile, and 10% methanol in acetonitrile. Fractions containing the product were combined and evaporated. The residue was titruated with diethyl ether (5×15 ml), filtered, and dried at 30° C. and 15 mm Hg to give 0.97 g (43%) tan powder, mp 62-67° C.

1. temperatureThe mixture was cooled to room temperature
2. customexcess benzyl alcohol was removed with a rotary evaporator at 0.12 mm Hg
3. customthe residue was purified by flash chromatography on a 160×55 mm silica gel 60 column
4. washeluted sequentially with acetonitrile, 50 methanol in acetonitrile, and 10% methanol in acetonitrile
5. additionFractions containing the product
6. customevaporated
7. filtrationfiltered
8. customdried at 30° C.