反应详情

A solution of tert-butyl (2S)-2-cyano-1-piperidinecarboxylate (13.10 g) [see Preparation 3] in methanol (500 ml) was added to a solution of hydroxylamine hydrochloride (21.6 g) and sodium carbonate (33.0 g) in water (600 ml). The reaction mixture was warmed to the reflux temperature and stirred for 8 hours after which time the methanol was removed under reduced pressure and the product extracted from the aqueous layer with ethyl acetate (3×500 ml). The combined organic layers were washed with water (500 ml), dried over magnesium sulphate and the solvent removed under reduced pressure to afford tert-butyl (Z)-(2S)-2-[amino(hydroxyimino)methyl]-1-piperidinecarboxylate (14.1 g) as a white solid.

1. temperatureThe reaction mixture was warmed to the reflux temperature
2. customwas removed under reduced pressure
3. extractionthe product extracted from the aqueous layer with ethyl acetate (3×500 ml)
4. washThe combined organic layers were washed with water (500 ml)
5. dry with materialdried over magnesium sulphate
6. customthe solvent removed under reduced pressure