Reacción #1509585

Ecuación de reacción

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

propynoic acid methyl ester

Dowtherm

→

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

Disolventes

DMF

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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.).

Fuente