反应详情

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.).

1. temperaturerefluxed for additional 1 h
2. customwas rised to 230° C
3. distillationDMF and MeOH were distilled off
4. temperatureThe reaction mixture was cooled down
5. additionEtOAc (200 ml) was added
6. filtrationthe resulting crystals were filtered off
7. washwashed with EtOAc and ether affording the title compound (44.8 g, FP>250° C.)