反应详情

0.8 g of 3,4-diaminothiophene dihydrobromide was added to a mixture of 0.74 g of N-ethyl-N,N-diisopropylamine in 40 ml of anhydrous THF, and the mixture was stirred at room temperature for 10 minutes, and then admixed with 0.58 g of 2-trifluoromethylphenyl isothiocyanate. The mixture was stirred at room temperature for 3 hours and at 40° C. for a further 10 minutes, and left to stand at room temperature overnight. After the solvent had been distilled off, the residue was admixed with water and extracted with ethyl acetate, and the insoluble fraction was filtered off. The organic phase was washed with water and dried over sodium sulfate, the solvent was distilled off and the residue was purified by column chromatography on silica gel using a mixture of 1 part by volume of toluene and 1 part by volume of ethyl acetate.

1. stirringThe mixture was stirred at room temperature for 3 hours and at 40° C. for a further 10 minutes
2. waitleft
3. waitto stand at room temperature overnight
4. distillationAfter the solvent had been distilled off
5. extractionextracted with ethyl acetate
6. filtrationthe insoluble fraction was filtered off
7. washThe organic phase was washed with water
8. dry with materialdried over sodium sulfate
9. distillationthe solvent was distilled off
10. customthe residue was purified by column chromatography on silica gel using
11. additiona mixture of 1 part by volume of toluene and 1 part by volume of ethyl acetate