反应详情

A mixture of sodium hydride (60% dispersion in mineral oil. 0.30 g), dimethyl diglycolate (0.81 g) and 4-[2-[N-(2-benzoxazolyl)-N-methylamino]ethoxy]benzaldehyde (2.22 g) in dry benzene (50 mL) was stirred at room temperature overnight. Acetic acid (1 mL) was added, the mixture was poured onto iced water and extracted with ethyl acetate. The combined ethyl acetate layers were washed with water, dried (MgSO4) and evaporated. The resulting oil was chromatographed on silica gel using 2% methanol in dichloromethane, and the product crystallised from ethyl acetate, mp 111°-112° C.

1. extractionextracted with ethyl acetate
2. washThe combined ethyl acetate layers were washed with water
3. dry with materialdried (MgSO4)
4. customevaporated
5. customThe resulting oil was chromatographed on silica gel using 2% methanol in dichloromethane
6. customthe product crystallised from ethyl acetate, mp 111°-112° C.