反应详情

To a solution of 6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepine of Example 1, Step B (3.0 g, 15.2 mmol) in dimethylformamide (35 mL) under nitrogen was added potassium carbonate (6.3 g, 45.6 mmol) followed by a solution of the crude 2,4difluorobenzoylchloride of Step A (22.8 mmol) in dimethylformamide (15 mL). After stirring at room temperature for 20 minutes, the reaction mixture was washed with water and stirred to give a solid which was collected by filtration. The solid was dissolved in chloroform and washed with 1 N sodium hydroxide and brine. The organic phase was dried over sodium sulfate and evaporated to dryness. The crude material was dissolved in dichloromethane and absorbed onto a silica Merck-60 flash column. Elution with 20% ethyl acetate in hexane provided the title compound (2.6 g, 51%) as a white foam which crystallized by sonication from hexane-ethanol, m.p. 161-163° C.

1. washthe reaction mixture was washed with water
2. stirringstirred
3. customto give a solid which
4. filtrationwas collected by filtration
5. dissolutionThe solid was dissolved in chloroform
6. washwashed with 1 N sodium hydroxide and brine
7. dry with materialThe organic phase was dried over sodium sulfate
8. customevaporated to dryness
9. dissolutionThe crude material was dissolved in dichloromethane
10. customabsorbed onto a silica Merck-60 flash column
11. washElution with 20% ethyl acetate in hexane