反应 #1509585

反应方程式

(E)-3-amino-but-2-enenitrile

propynoic acid methyl ester

Dowtherm

→

2-Methyl-6-oxo-1,6-dihydro-pyridine-3-carbonitrile

溶剂

DMF

反应条件

后处理

1. 1
   温度refluxed for additional 1 h
2. 2
   其他was rised to 230° C
3. 3
   workup.DISTILLATIONDMF and MeOH were distilled off
4. 4
   温度The reaction mixture was cooled down
5. 5
   workup.ADDITIONEtOAc (200 ml) was added
6. 6
   过滤the resulting crystals were filtered off
7. 7
   洗涤washed with EtOAc and ether affording the title compound (44.8 g, FP>250° C.)

实验过程

A solution of (E)-3-amino-but-2-enenitrile (100 g) and propynoic acid methyl ester in DMF (200 ml) was stirred at 25° C. for 2 h and refluxed for additional 1 h. Dowtherm (100 ml) was added and the temperature was rised to 230° C. DMF and MeOH were distilled off. The reaction mixture was cooled down, EtOAc (200 ml) was added and the resulting crystals were filtered off and washed with EtOAc and ether affording the title compound (44.8 g, FP>250° C.).

来源