四正丙氧基甲烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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. is directly distilled out of the reaction flask After completion of the reaction, excess tetra-n-propylorthocarbonate is distilled off under reduced pressure the resulting raw material purified by column chromatography over silica gel (eluant: hexane/tert.butylmethyl ether 6:1)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a small distillation apparatus 2.5 g (9.8 mmol) of 2-amino-5-chloro-N,N′-dipropylbenzamidine and 3.4 g (13.8 mmol) tetra-n-propylorthocarbonate are heated at 135° C. for 14 hours. Then propanol and excess tetra-n-propylorthocarbonate are distilled off in a water jet vacuum and the residue is purified by column chromatography on silica gel (eluant: hexane/tert.butylmethylether 10:1). Yield: 1.1 g of (6-chloro-2-propoxy-3-propyl-3H-quinazolidine-4-ylidene)propylamine in the form of brownish crystals, m.p. 50-51° C. Then propanol and excess tetra-n-propylorthocarbonate are distilled off in a water jet vacuum the residue is purified by column chromatography on silica gel (eluant: hexane/tert.butylmethylether 10:1)