反应详情

To a solution of [1-(1-cyano-cyclopropylcarbamoyl)-cyclopropyl]-carbamic acid tert-butyl ester (250 mg, 0.942 mmol) in anhydrous EtOH (2.4 mL) was added NaOEt (21 wt % in EtOH, 0.70 mL, 1.9 mmol) via syringe in one portion. The orange reaction was stirred for 1 h. To the orange solution was added solid NH4Cl (202 mg, 3.77 mmol) and NH3 (7M in MeOH, 0.14 mL, 0.94 mmol). The reaction vial was sealed and stirred at room temperature for 15 h. The resulting suspension was filtered rinsing with EtOH. The filtrate was concentrated and the resulting solids were triturated with EtOAc to give 182 mg of [1-(1-carbamimidoyl-cyclopropylcarbamoyl)-cyclopropyl]-carbamic acid tert-butyl ester hydrochloride as a white solid, m/z 283.6 [M+H]+.

1. customThe orange reaction
2. customThe reaction
3. customvial was sealed
4. stirringstirred at room temperature for 15 h
5. filtrationThe resulting suspension was filtered
6. washrinsing with EtOH
7. concentrationThe filtrate was concentrated
8. customthe resulting solids were triturated with EtOAc