反应详情

温度

100 °C

Methyl (2S)-1-[(cyclohexylmethyl)sulfonyl]-2-piperidinecarboxylate (3.0 g) [see Preparation 25) was dissolved in 1,4-dioxane (30 ml) and 0.88 aqueous ammonia solution (25 ml) was added. Ammonia gas was bubbled through the mixture for 20 mins. and the reaction mixture was heated to 100° C. in a sealed vessel for 56 hours. After this time the mixture was cooled and the solvent removed under reduced pressure. The residue was taken up in ethyl acetate and washed with saturated aqueous sodium hydrogen carbonate solution, brine, dried over magnesium sulphate and the solvent was removed under reduced pressure to afford (2S)-1-[(cyclohexylmethyl)sulfonyl]-2-piperidinecarboxamide (1.77 g) as a colourless oil.

1. customPreparation 25)
2. customAmmonia gas was bubbled through the mixture for 20 mins
3. temperatureAfter this time the mixture was cooled
4. customthe solvent removed under reduced pressure
5. washwashed with saturated aqueous sodium hydrogen carbonate solution, brine
6. dry with materialdried over magnesium sulphate
7. customthe solvent was removed under reduced pressure