反应详情

温度

60 °C

A mixture of ethyl 1,2-dihydro-1-oxophthalazin-4-ylacetate (11.5 g.) and sodium hydride (2.7 g.; 50% w/w dispersion in mineral oil) in dimethylformamide (125 ml.) was stirred at 60° C. for 1 hour under nitrogen. The solution obtained was cooled to room temperature and then 4-bromo-3-chlorobenzyl bromide (15.0 g.) was added, and the mixture stirred at 60° C. for 2 hours. After cooling to 25° C. the reaction mixture was poured into water (500 ml.). The aqueous mixture obtained was extracted with ethyl acetate (400 ml.). The extracts were washed with water, dried (MgSO4), and evaporated to give a solid, which was crystallised from propan-2-ol to yield ethyl 2-(3-chloro-4-bromobenzyl)-1,2-dihydro-1-oxophthalazin-4-ylacetate (7.3 g.), m.p. 142°-145° C.

1. customThe solution obtained
2. temperaturewas cooled to room temperature
3. stirringthe mixture stirred at 60° C. for 2 hours
4. temperatureAfter cooling to 25° C. the reaction mixture
5. customThe aqueous mixture obtained
6. extractionwas extracted with ethyl acetate (400 ml.)
7. washThe extracts were washed with water
8. dry with materialdried (MgSO4)
9. customevaporated
10. customto give a solid, which
11. customwas crystallised from propan-2-ol