反应详情

(1-Cyano-cyclopropyl)-carbamic acid tert-butyl ester (2.44 g, 13.40 mmol) was dissolved in dry EtOH (33 mL). Sodium ethoxide (21 wt % in EtOH solution, 10.70 mL, 22.80 mmol)) was added and the reaction was stirred for 1 h at room temperature under an atmosphere of dry argon. To the light yellow solution was added solid NH4Cl (2.94 g, 55 mmol) followed by 7 M NH3 in MeOH (8.08 mL, 56.60 mmol). The reaction was capped and allowed to stir for 16 h. The turbid suspension was filtered using MeOH to rinse. The filtrate was concentrated in vacuo and the solid residue was re-suspended in dry EtOH. The solids were filtered off, rinsing with EtOH. The filtrate was concentrated to give 2.91 g of (1-Carbamimidoyl-cyclopropyl)-carbamic acid tert-butyl ester as a light yellow solid. m/z 200.48 [M+1]+

1. customThe reaction was capped
2. stirringto stir for 16 h
3. filtrationThe turbid suspension was filtered
4. washto rinse
5. concentrationThe filtrate was concentrated in vacuo
6. filtrationThe solids were filtered off
7. washrinsing with EtOH
8. concentrationThe filtrate was concentrated