反应详情

A suspension of 2-amino-5-bromobenzonitrile (58.5 g, 297 mmol) in ethyl chloroformate (141 mL, 1.48 mol) was heated at reflux for 5 h. The excess ethyl chloroformate (99 mL) was distilled off and toluene (96 mL) was added. Slow addition of cyclohexane (228 mL) induced crystallization. The resulting solid was collected by filtration and rinsed with cyclohexane. Drying in vacuo afforded the title compound (54.3 g, 68%) as an orange solid. MS: m/e=267.1/269.2 [M—H−].

1. temperaturewas heated
2. temperatureat reflux for 5 h
3. distillationThe excess ethyl chloroformate (99 mL) was distilled off
4. additiontoluene (96 mL) was added
5. additionSlow addition of cyclohexane (228 mL)
6. customcrystallization
7. filtrationThe resulting solid was collected by filtration
8. washrinsed with cyclohexane
9. customDrying in vacuo