反应详情

2-Oxo-3-tert-butoxycarbonylamino-5-pivaloyl-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (4.00 g) obtained from Step 1 of Example 89 was suspended in toluene (56 ml), 2-bromo-2′-methylacetophenone (2.72 g), 1N aqueous sodium hydroxide (28 ml) and tetra n-butylammonium bromide (40 mg) were added, and the mixture was stirred overnight at room temperature. The reaction mixture was weakly acidified with 1N hydrochloric acid, extracted with methylene chloride. The organic layer was washed with saturated aqueous sodium bicarbonate, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. Diisopropyl ether was added to the residue for trituration, collected by filtration, to thereby obtain 4.54 g of the titled compound.

1. extractionextracted with methylene chloride
2. washThe organic layer was washed with saturated aqueous sodium bicarbonate
3. dry with materialdried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. additionDiisopropyl ether was added to the residue for trituration
6. filtrationcollected by filtration