反应详情

温度

85 °C

Ethyl 4-bromobenzimidate hydrochloride (35.6 g, 135 mmol), formic hydrazide (16.16 g, 269 mmol) and triethylamine (75 mL, 538 mmol) were combined in a screw capped flask and heated to 85° C. for 16 h. The solution was condensed under reduced pressure to afford a solid, which was partitioned between water and ethyl acetate (3×), dried over magnesium sulfate and solvent removed under reduced pressure. The resulting solid was sonicated with 20% ethyl acetate in hexanes, filtered and dried to afford the title compound (14.6 g, 65.2 mmol, 48% yield). MS (ESI) m/z 224.1 [M]+, 226.1 [M+2]+.

1. customcapped flask
2. customcondensed under reduced pressure
3. customto afford a solid, which
4. customwas partitioned between water and ethyl acetate (3×)
5. dry with materialdried over magnesium sulfate and solvent
6. customremoved under reduced pressure
7. customThe resulting solid was sonicated with 20% ethyl acetate in hexanes
8. filtrationfiltered
9. customdried