反应详情

4-[2-Hydroxy-3-(N,N dibenzylamino)propoxy]-1,3-dihydro-2H-benzimidazol-2-one (4.35 g, 10.8 mrol) was dissolved in methanol (200 mL) and treated with a vast excess of ammonium formate (13.0 g, 0.21 mol), followed by 10% palladium on carbon (1.5 g). The suspension was stirred at reflux for 3 hours. After cooling the suspension, the reaction mixture was filtered through Celite. The filtrate concentrated in vacuo to a pale brown oil which slowly crystallized upon standing. The resulting solid was triturated using chloroform containing methanol and filtered to give 1.56 g (65%) as the desired product of a pale grey solid. NMR. MS.

1. temperatureat reflux for 3 hours
2. temperatureAfter cooling the suspension
3. filtrationthe reaction mixture was filtered through Celite
4. concentrationThe filtrate concentrated in vacuo to a pale brown oil which
5. customslowly crystallized
6. customThe resulting solid was triturated
7. additioncontaining methanol
8. filtrationfiltered