反应详情

温度

5 °C

(S)-Benzyl-3-(tert-butyl dimethylsilyloxy)glutaramate (100 g) was dissolved in ethyl acetate and placed in pressure flask. To this Palladium on charcoal (5%, 1 g) was added and stirred under hydrogen atmosphere (˜2.8 Kg). Palladium was removed by filtration. The filtrate was mixed with water and adjusted pH to ˜9.0 by using Aq ammonia solution. The reaction mass was stirred and layers were separated. The aqueous phase was washed with dichloromethane and dichloromethane was added to aqueous phase. The reaction mass was cooled to 5° C. and pH was adjusted to 4.0 with Aq phosphoric acid. The reaction mass was stirred and layers were separated. The organic phase was washed with water and dried over sodium sulphate. The organic layer was evaporated under vacuum to yield residue. Residue was dissolved in dichloromethane and to this solution heptane was added, stirred, filtered and dried to yield (S)-3-(tert-butyl dimethylsilyloxy)glutaric acid monoamide.

1. customplaced in pressure flask
2. customPalladium was removed by filtration
3. additionThe filtrate was mixed with water and adjusted pH to ˜9.0
4. stirringThe reaction mass was stirred
5. customlayers were separated
6. washThe aqueous phase was washed with dichloromethane and dichloromethane
7. additionwas added to aqueous phase
8. stirringThe reaction mass was stirred
9. customlayers were separated
10. washThe organic phase was washed with water
11. dry with materialdried over sodium sulphate
12. customThe organic layer was evaporated under vacuum
13. customto yield residue
14. additionwas added
15. stirringstirred
16. filtrationfiltered
17. customdried