HRID913009
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 135 °C
PROCEDURE
实验过程
A suspension of 5-benzyloxy-1-methyl-4-oxo-1,4-dihydro-pyridine-2-carboxylic acid (18.2 g, 70.2 mmol) in 100 mL of DMF was stirred at oil bath temperature (130-140° C.) for 1.5 h. The reaction mixture was concentrated in vacuo, and the residual oil was diluted with dichloromethane (10 mL) and ethyl acetate (80 mL). The precipitated solid was collected by suction filtration to give 3-benzyloxy-1-methyl-1H-pyridin-4-one as a yellow powder (14.2 g, 94% yield). MS-ESI (m/z): 215.7 [M+1]+, 91.2.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- additionthe residual oil was diluted with dichloromethane (10 mL) and ethyl acetate (80 mL)
- filtrationThe precipitated solid was collected by suction filtration