反应详情

A mixture of 1.87 g of 3,4-diaminothiophene dihydrochloride, 60 ml of anhydrous THF and 2.58 g of N-ethyl-N,N-diisopropylamine was stirred at room temperature for 30 minutes and then admixed with 2.04 g of 2,6-dichlorophenyl isothiocyanate. After the mixture had been heated to 40° C. for 10 minutes, it was stirred at room temperature for approx. 18 hours, and the solvent was distilled off, and the residue admixed with water and extracted repeatedly with ethyl acetate. After the combined organic phases had been treated with activated carbon, they were dried over sodium sulfate and the solvent was again distilled off. A crystalline solid was obtained and, after stirring with a little ethyl acetate, was filtered off. M.p. 165° C.

1. temperatureAfter the mixture had been heated to 40° C. for 10 minutes
2. stirringit was stirred at room temperature for approx. 18 hours
3. distillationthe solvent was distilled off
4. extractionthe residue admixed with water and extracted repeatedly with ethyl acetate
5. additionAfter the combined organic phases had been treated with activated carbon, they
6. dry with materialwere dried over sodium sulfate
7. distillationthe solvent was again distilled off
8. customA crystalline solid was obtained
9. filtrationwas filtered off