反应详情

Stir a mixture of dichloroethane (500 mL), N-amino-4-hydroxypiperidine (10.66 g, 91.88 mmol), (R)-4-((R)-4-benzyl-2-oxo-oxazolidin-3-yl)-3-(4-benzyloxy-2,6-dichloro-benzyl)-4-oxo-butyraldehyde (40.2 g, 76.57 mmol) and sodium triacetoxyborohydride (48.47 g, 229.71 mmol) at room temperature for 21 hours. Bring the reaction to 55° C. and is stir for 1 hour. Cool the reaction, dilute with dichloromethane, and wash with water. Dry the organic layer (Na2SO4), remove the solvent in vacuo to afford crude product, and purify on silica with a 100% ethyl acetate and 10% methanol in methylene chloride to afford 30 g (90%) of the titled product. MS (m/z): 449 (M+).

1. customBring the reaction to 55° C.
2. stirringis stir for 1 hour
3. temperatureCool
4. customthe reaction
5. washwash with water
6. dry with materialDry the organic layer (Na2SO4)
7. customremove the solvent in vacuo
8. customto afford crude product
9. custompurify on silica with a 100% ethyl acetate and 10% methanol in methylene chloride