反应详情

A 10 mL reaction flask was charged with 3-(2-Amino-ethyl)-1-(2-isopropyl-5-methyl-cyclohexanecarbonyl)-5-methylsulfanyl-1,3-dihydro-benzoimidazol-2-one (Compound #42, 300 mg) and 1% TFA/DMSO (1 mL). Oxygen was bubbled through the reaction mixture for 20 min and sealed. The reaction mixture was stirred for 18 h and crude product was purified by preparative HPLC (Ultro 120 (10 um) C18Q) using a 40-60% acetonitrile/H2O (with 0.1% TFA) gradient. The pure fractions were combined, concentrated and lyophilized to give a light fluffy colorless solid (296 mg 94%). MS (ESI) m/z 406 (M++1).

1. customA 10 mL reaction flask
2. customOxygen was bubbled through the reaction mixture for 20 min
3. customsealed
4. customcrude product was purified by preparative HPLC (Ultro 120 (10 um) C18Q)
5. concentrationconcentrated
6. customto give a light fluffy colorless solid (296 mg 94%)