反应详情

Alternately, combine 1-(t-butoxycarbonyl)-4-(1H-benzimidazol-2-yl)[1,4]diazepane (1.7 g, 5.37 mmol) and dimethylformamide (40 mL). Add sodium hydride (0.23 g, 60% n in oil, 5.75 mmol). After 15 minutes, add 4-fluorobenzyl bromide (0.73 mL, 5.86 mmol). After 18 hours, partition the reaction mixture between dichloromethane and a saturated aqueous sodium bicarbonate solution. Separate the layers and extract the organic layer five times with water and then brine. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give 1-(t-butoxycarbonyl)-4-(1-(4-fluorobenzyl-1H-benzimidazol-2-yl)[1,4]diazepane: Rf=0.42 (silica gel, 50% ethyl acetate/hexane).

1. waitAfter 18 hours
2. custompartition the reaction mixture between dichloromethane
3. customSeparate the layers
4. extractionextract the organic layer five times with water
5. dry with materialDry the organic layer over Na2SO4
6. filtrationfilter
7. customevaporate in vacuo