反应 #66095

反应方程式

sodium bicarbonate

Ethyl isonipecotate

formic acid

formaldehyde

→

1-methyl-piperidine-4-carboxylic acid ethyl ester

收率 61.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   温度the mixture was heated
2. 2
   温度at reflux for 24 h
3. 3
   温度After cooling
4. 4
   浓缩the mixture was concentrated in vacuo
5. 5
   其他to give an oil which
6. 6
   过滤then filtered
7. 7
   浓缩The filtrate was concentrated in vacuo

实验过程

Ethyl isonipecotate (3.0 g, 19.1 mmol) was added to a mixture of 90% formic acid (10 mL) and 30% aqueous formaldehyde (10 mL, 100 mmol) then the mixture was heated at reflux for 24 h. After cooling, the mixture was concentrated in vacuo to give an oil which was dissolved in dichloromethane. Solid sodium bicarbonate (1 g) was added and the mixture stirred for 1 h then filtered. The filtrate was concentrated in vacuo to afford 1-methyl-piperidine-4-carboxylic acid ethyl ester (2.0 g, 61%) as a liquid, which was used as such for the next step.

来源