反应详情

To a solution of (3RS)-1-{(3-azabicyclo[3.2.2]non-3-yl)-carbonylmethyl}-3-amino-5-(2-fluorophenyl)-2,3-dihydro-1H-1,4-benzodiazepin-2-one (100mg) and 4-nitrophenyl N-(3-trifluoromethylphenyl)carbamate (90.1 mg) in dimethylformamide (2 ml) was added triethylamine (28 mg) under stirring at ambient temperature. The mixture was stirred for 3.5 hours under the same condition. The reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed with water three times and dried over magnesium sulfate. The solvent was removed in vacuo to give an amorphous mass, which was pulverized in diisopropyl ether under vigorous stirring. The resulting powder was collected by filtration and washed with diisopropyl ether to afford N-[(3RS)-1-{(3-azabicyclo[3.2.2]non-3-yl)-carbonylmethyl}-2,3-dihydro-5-(2-fluorophenyl)-2-oxo-1H-1,4-benzodiazepin-3-yl]-N'-(3-trifluoromethylphenyl)urea (124.4 mg).

1. stirringThe mixture was stirred for 3.5 hours under the same condition
2. extractionextracted with ethyl acetate
3. washThe extract was washed with water three times
4. dry with materialdried over magnesium sulfate
5. customThe solvent was removed in vacuo
6. customto give an amorphous mass, which
7. filtrationThe resulting powder was collected by filtration
8. washwashed with diisopropyl ether