反应详情

Add in one portion 1,1′-carbonyldiimidazole (8.3 g, 51 mmol) to a solution of pyrrolidine-1,3-dicarboxylic acid 1-tert-butyl ester (10.0 g, 46.5 mmol) in dichloromethane (155 mL) at RT. Allow the mixture to stir for 15 min. Add slowly N,O-dimethylhydroxylamine hydrochloride (5.4 g, 55.8 mmol). Stir the reaction mixture at RT overnight. Dilute the mixture with dichloromethane (200 mL), wash with water (2×300 mL), brine (200 mL), dry over Na2SO4, filter, and concentrate. Purify the crude material by flash chromatograph and elute with 50-100% ethylacetate/hexane to give 10.8 g (90%) of the title compound. LC-MS/ES m/z 203.0 [M-tert-Bu+H]+.

1. stirringStir the reaction mixture at RT overnight
2. washwash with water (2×300 mL), brine (200 mL)
3. dry with materialdry over Na2SO4
4. filtrationfilter
5. concentrationconcentrate
6. customPurify the crude material by flash chromatograph
7. washelute with 50-100% ethylacetate/hexane