反应详情

A solution of 7.1 g of the ethyl 5-aminosulfonyl-2,2-dimethylvalerate obtained in Reference Example 26 in 20 ml of tetrahydrofuran was added dropwise to a suspension of 1.71 g of lithium aluminum hydride in 100 ml of tetrahydrofuran with ice-cooling and stirring. After completion of dropwise addition, the mixture was stirred at 0° C. for 40 minutes and after addition of aqueous tetrahydrofuran for decomposition of excess lithium aluminum hydride, 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 (100 g) column chromatography and elution was carried out with hexane-ethyl acetate (4:1) to provide 3.39 g of the title compound as oil.

1. temperaturecooling
2. additionAfter completion of dropwise addition
3. stirringthe mixture was stirred at 0° C. for 40 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 (100 g) column chromatography and elution