反应详情

A solution of 5 g (20 mmol) of methyl (S)-2-amino-3-tert-butoxycarbonylaminopropanoate hydrochloride and 4.3 g (20 mmol) of N,N-bis(2-chloroethyl)methanesulphonamide in 65 ml of N,N-diisopropylethylamine is heated at 127° C. with vigorous stirring for 18 h. After addition of water, the product is extracted with ethyl acetate. The organic phases are combined, washed with water, dried over magnesium sulphate, filtered and concentrated under vacuum. The crude product obtained is purified by chromatography over silica gel eluted with a 50/50 heptane/ethyl acetate mixture. 3.3 g (46%) of methyl (S)-3-tert-butoxycarbonylamino-2-(4-methanesulphonylpiperazin-1-yl)propanoate are obtained in the form of a white solid.

1. extractionthe product is extracted with ethyl acetate
2. washwashed with water
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customThe crude product obtained
7. customis purified by chromatography over silica gel
8. washeluted with a 50/50 heptane/ethyl acetate mixture