反応 #1509585

反応方程式

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

propynoic acid methyl ester

Dowtherm

→

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

溶媒

DMF

反応条件

後処理

1. 1
   温度refluxed for additional 1 h
2. 2
   その他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
   ろ過the resulting crystals were filtered off
7. 7
   洗浄washed with EtOAc and ether affording the title compound (44.8 g, FP>250° C.)

実験手順

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.).

出典