反应详情

温度

50 °C

Methanol (20 ml) and 10% palladium carbon (68 mg) were added to 1-(1-tert-butylcarbonylmethyl-2-oxo-5-phenyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl)-3-(3-benzyloxycarbonylphenyl)urea (635 mg), the mixture was stirred at 50° C. under hydrogen atmosphere for 2 hours. The reaction mixture was filtrated, the filtrate was concentrated under reduced pressure. The residue was dissolved in 2 N aqueous sodium hydroxide, washed with ether, adjusted to pH 2 with concentrated hydrochloric acid, and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under the pressure, the mixed solvent of isopropyl ether and ethyl acetate was added to the residue for trituration, and collected by filtration, to thereby obtain 144 mg of the title compound as a colorless solid.

1. filtrationThe reaction mixture was filtrated
2. concentrationthe filtrate was concentrated under reduced pressure
3. dissolutionThe residue was dissolved in 2 N aqueous sodium hydroxide
4. washwashed with ether
5. extractionextracted with chloroform
6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
7. customThe solvent was evaporated under the pressure
8. additionthe mixed solvent of isopropyl ether and ethyl acetate was added to the residue for trituration
9. filtrationcollected by filtration