反应详情

6-tert-butyl 5-methyl 5-methyl-6-azaspiro[2.5]octane-5,6-dicarboxylate (D5) (320 mg, 1.13 mmol) was partitioned between dioxane/water (8/8 ml) prior addition of LiOH H2O (190 mg, 4.52 mmol). The mixture was stirred at RT for 18 hrs then heated at 150° C. under microwave irradiation 40 min (4 cycles of 10 min each). Organic solvent was evaporated off and the aqueous solution washed with EtOAc (2×10 ml), acidified to pH˜4 with citric acid sat. sol. and extracted with EtOAc (3×10 ml). The organic phases were washed with NaCl sat. sol, dried over Na2SO4 and evaporated to reduced pressure to afford the title compound (D6) (114 mg).

1. temperaturethen heated at 150° C. under microwave irradiation 40 min (4 cycles of 10 min each)
2. customOrganic solvent was evaporated off
3. washthe aqueous solution washed with EtOAc (2×10 ml)
4. extractionextracted with EtOAc (3×10 ml)
5. washThe organic phases were washed with NaCl sat. sol
6. dry with materialdried over Na2SO4
7. customevaporated to reduced pressure