反应详情

In a small distillation apparatus a mixture of 12.4 g(0.1 mol) 2-amino-3-cyanothiophene and 37.2 g (0.15 mol) tetra-n-propylorthocarbonate is heated for 3 hours at 155° C. n-PrOH, which arises during the reaction is directly distilled out of the reaction flask. After completion of the reaction, excess tetra-n-propylorthocarbonate is distilled off under reduced pressure and the resulting raw material purified by column chromatography over silica gel (eluant: hexane/tert.butylmethyl ether 6:1). Yield: 10.6 g of 3-cyano-2-(1,1-dipropoxymethyleneamino)thiophene in the form of slightly brownish crystals; m.p. 65-67° C.

1. distillationis directly distilled out of the reaction flask
2. customAfter completion of the reaction, excess tetra-n-propylorthocarbonate
3. distillationis distilled off under reduced pressure
4. customthe resulting raw material purified by column chromatography over silica gel (eluant: hexane/tert.butylmethyl ether 6:1)