反应 #2195505
ord-e71af8df398141858e4518bc0f82dc60
反应方程式
4-(tert-butyldimethylsilyloxy)dihydro-2H-pyran-2,6(3H)-dione
ammonium hydroxide
ammonia
→
title compound
4-(tert-Butyldimethylsilyloxy)piperidine-2,6-dione
溶剂
反应条件
温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度Cool in an ice/water bath
- 2其他Cap the pressure tube
- 3温度Cool the mixture
- 4浓缩concentrate in vacuo
- 5其他Purify the residue by silica gel chromatography
实验过程
Dissolve 4.1 mmol of 4-(tert-butyldimethylsilyloxy)dihydro-2H-pyran-2,6(3H)-dione (Nagao Y et al., Chem. Lett. 1990 9: 1503) in 10 mL of dioxane in a pressure tube. Cool in an ice/water bath, add 15 mL of saturated ammonium hydroxide and treat with gaseous ammonia via bubbler for about 10 min. Cap the pressure tube and heat in a 100° C. oil bath for 17 h. Cool the mixture and concentrate in vacuo. Purify the residue by silica gel chromatography using ethyl acetate/hexanes eluant to yield the title compound.