HRID1249599
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A suspension of 5-(benzyloxy)-1,4-dihydro-4-oxo-2-pyridinecarboxylic acid (8.24 g, 33.6 mmole) in 120 ml of ethanol was cooled to 0° C. and treated with a stream of dry HCl for 15 minutes. The resulting mixture was heated at 50° C. for 5.5 hours. The volatiles were removed in vacuo and the residue was treated with water. While cooling, the pH was raised to 7 with saturated potassium bicarbonate and the resulting mixture was extracted with dichloromethane. The extracts were washed with brine and dried over sodium sulfate. Filtration and concentration in vacuo produced 7.32 g of the title compound.
WORKUP
后处理
- temperatureThe resulting mixture was heated at 50° C. for 5.5 hours
- customThe volatiles were removed in vacuo
- additionthe residue was treated with water
- temperatureWhile cooling
- temperaturethe pH was raised to 7 with saturated potassium bicarbonate
- extractionthe resulting mixture was extracted with dichloromethane
- washThe extracts were washed with brine
- dry with materialdried over sodium sulfate
- filtrationFiltration and concentration in vacuo