反应详情

515 Milligrams of diethyl 5-amino-3-methylthiophene-2,4-dicarboxylate and 296 mg of 3-thiopheneacetonitrile were added to 8 mL of 4N hydrogen chloride-dioxane solution and stirred for 10 hours. Thereafter the liquid reaction mixture was poured on ice, and its pH was adjusted to 8-9 with 25% aqueous ammonia. Whereupon precipitated crystals were recovered by filtration and washed first with water, and then with hexane. The crude crystals were recrystallized from a liquid mixture of N,N-dimethylformamide and cyclohexane, to provide 397 mg of the title compound.

1. customThereafter the liquid reaction mixture
2. additionwas poured on ice, and its pH
3. customWhereupon precipitated crystals
4. filtrationwere recovered by filtration
5. washwashed first with water
6. customThe crude crystals were recrystallized from a liquid mixture of N,N-dimethylformamide and cyclohexane