反应详情

温度

80 °C

Combine 1-methyl-4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (1.79 g, 5.9 mmol) and ethyl chloroformate (0.75 mL, 7.8 mmol) in toluene (20 mL). Heat to 80° C. After 2 hours, cool the reaction mixture and dilute with ethyl acetate. Extract with a saturated aqueous sodium bicarbonate solution, dry the organic layer over MgSO4, filter, and evaporate in vacuo to give 1-ethoxycarbonyl-4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl)[1,4]diazepane: Rf=0.87 (silica gel, dichloromethane/methanol, 90/10).

1. temperaturecool the reaction mixture
2. extractionExtract with a saturated aqueous sodium bicarbonate solution
3. dry with materialdry the organic layer over MgSO4
4. filtrationfilter
5. customevaporate in vacuo