反应详情

While a suspension of 0.35 g of lithium aluminum hydride in 30 ml of tetrahydrofuran was stirred with ice-cooling, a solution of 1.5 g of ethyl 4-aminosulfonyl-2,2-dimethylbutyrate in 8 ml of tetrahydrofuran was added dropwise. After completion of dropwise addition, the mixture was stirred at 0° C. for 30 minutes and, then, at room temperature for 30 minutes. To this reaction mixture was added aqueous tetrahydrofuran for decomposition of excess lithium aluminum hydride and the mixture was neutralized with 2N-hydrochloric acid and extracted with ethyl acetate. The extract was washed with water and dried (MgSO4) and the solvent was distilled off. The residue was subjected to silica gel column chromatography and elution was carried out with hexane-ethyl acetate (1:1) to provide 0.94 g of the title compound. m.p.: 75°-76° C.

1. temperaturecooling
2. additionAfter completion of dropwise addition
3. stirringthe mixture was stirred at 0° C. for 30 minutes
4. extractionextracted with ethyl acetate
5. washThe extract was washed with water
6. dry with materialdried (MgSO4)
7. distillationthe solvent was distilled off
8. washThe residue was subjected to silica gel column chromatography and elution