Реакция #1509585

Уравнение реакции

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

propynoic acid methyl ester

Dowtherm

→

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

Растворители

DMF

Условия реакции

Обработка

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

Методика

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.).

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