反应详情

1.1 g of 1,3,5-trimethyl-N-(1,1,3-trimethyl-4-indanyl)pyrazole-4-carboxamide, 0.79 g of phosphorus pentasulfide and 15 ml of hexamethylphosphoramide (HMPA) were stirred at 100° C. for 8 hours. After cooling, the reaction mixture was poured into ice water and extracted with ether. The extracts ether layer were dried over anhydrous magnesium sulfate and then the solvent was distilled off. The residue was chromatographed on silica gel to obtain 0.75 g of 1,3,5-trimethyl-N-(1,1,3-trimethylindane-4-yl)pyrazole-4-carbothioamide (yield 65%).

1. temperatureAfter cooling
2. extractionextracted with ether
3. dry with materialThe extracts ether layer were dried over anhydrous magnesium sulfate
4. distillationthe solvent was distilled off
5. customThe residue was chromatographed on silica gel