反应详情

温度

50 °C

To a stirred solution of 5-cyclohexyl-1,3-dihydro-1-methyl-3(R,S)-[(4-nitrophenyloxycarbonyl)amino]-2H-1,4-benzodiazepin-2-one (150 mg, 0.34 mmol) [Example 11, Step 3], in anhydrous dimethylformamide (3 ml) was added triethylamine (48 μl, 0.34 mmol). After 5 min a solution of 5-(3-aminophenyl)-2methyltetrazole (65 mg, 0.37 mmol) in anhydrous dimethylformamide (3m]) was added, and the solution heated at 50° C. for 2 h. After this time the solution was cooled to ambient temperature and evaporated in vacuo. The residue was dissolved in ethyl acetate (5 ml) and on standing a solid precipitated. This was recrystallised from ethyl acetate to afford the urea (65 mg, 40%) as a colourless solid. mp 195°-196° C. 1H NMR (360 MHz, CDCl3) δ 1.05-2.06 (10H, m), 2.79 (1H, m), 3.45 (3H, s), 4.36 (3H, s), 5.42 (1H, d, J=8 Hz), 6.75 (1H, d, J=8 Hz), 7.15-7.60 (7H, m), 7.77 (1H, d, J=8 Hz), 8.06 (1H, s).

1. temperatureAfter this time the solution was cooled to ambient temperature
2. customevaporated in vacuo
3. dissolutionThe residue was dissolved in ethyl acetate (5 ml)
4. customprecipitated
5. customThis was recrystallised from ethyl acetate