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温度

0 °C

A mixture of alcohol from Example 26 (63 mg, 0.194 mmole) 4-dimethylaminopyridine (78 mg, 0.639 mmole) , acetic anhydride (0.06 ml, 0.639 mmole) in dichloromethane (10 ml) was stirred at 0° C. for 8 hours. The volatiles were removed and the crude mixture applied directly to a silica gel column and eluted with 5% methanol in chloroform (Rf =0.34). The product slowly crystallized from hexane-ethyl acetate at 0° C. to give 41 mg of colorless cubes, m.p. 107°-110° C. after filtration. IR (KBr): 1702 cm-1. High Res. Mass Spec. Calcd. for C20H21N3O4 : 368.1610 (M+H) . Found: 368.1611.

1. customThe volatiles were removed
2. washeluted with 5% methanol in chloroform (Rf =0.34)
3. customThe product slowly crystallized from hexane-ethyl acetate at 0° C.
4. customto give 41 mg of colorless cubes, m.p. 107°-110° C.
5. filtrationafter filtration