反应详情

To a solution of 113.2 g (0.2 mole) of tert-butyl 4-benzyloxycarbonyl-8-methyl-alpha-phthalimido-1-thia-3,8-diazaspiro[4.5]decane-2-acetate (obtained in 3.1) in 730 ml of dioxan are added 13.4 g of hydrazine hydrate. After 24 hours, a further 6 g of hydrazine hydrate are added, followed by filtration after 24 hours. The mixture is evaporated and the residue is dissolved in 1 liter of benzene, then filtered after 24 hours and the new residue obtained by evaporation is passed through a column of silica gel (60 Merck), using a 91 v/v benzene-methanol mixture as eluent. In this way, a solution of tert-butyl alpha-amino-4-benzyloxycarbonyl-8-methyl-1-thia-3,8-diazaspiro[4.5]decane-2-acetate is obtained, which is subjected as much to step 5.1.

1. filtrationfollowed by filtration after 24 hours
2. customThe mixture is evaporated
3. dissolutionthe residue is dissolved in 1 liter of benzene
4. filtrationfiltered after 24 hours
5. customthe new residue obtained by evaporation