반응 #1509585

반응 방정식

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

propynoic acid methyl ester

Dowtherm

→

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

용매

DMF

반응 조건

후처리

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

실험 절차

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.).

출처