反应详情

The mixture of 8, 11-dichlorodibenz[b,f][1,4]oxazepine (0.32 g, 1.19 mmol), 1-nonylpiperazine (0.38 g, 1.79 mmol) and 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU) (0.72 mL, 0.73 g, 4.77 mmol) in acetonitrile (15 mL) was heated at reflux for 6 h. After the mixture was concentrated, water (20 mL) and ethyl acetate (20 mL) were added. The two phases were separated and the aqueous phase was extracted with ethyl acetate (2×20 mL). The combined ethyl acetate solution was dried over magnesium sulfate and filtered. The filtrate was then concentrated in vacuo to dryness and the residue was subjected to column chromatography using ethyl acetate/hexane (1/2) as the eluent. The title compound was obtained as a white solid (0.15 g, 28%), m.p. 64°-66° C., MS 440 (M+ +1).

1. temperaturewas heated
2. temperatureat reflux for 6 h
3. concentrationAfter the mixture was concentrated
4. additionwater (20 mL) and ethyl acetate (20 mL) were added
5. customThe two phases were separated
6. extractionthe aqueous phase was extracted with ethyl acetate (2×20 mL)
7. dry with materialThe combined ethyl acetate solution was dried over magnesium sulfate
8. filtrationfiltered
9. concentrationThe filtrate was then concentrated in vacuo to dryness