反应详情

A mixture of 4-(amino(6-oxo-2-(3-(trifluoromethyl)phenylamino)cyclohex-1-enyl)methyl)-3-methylbenzonitrile hydrochloride (intermediate 52, 1.06 g, 2.43 mmol), 1,1-carbonyl-diimidazole (495 mg, 3.05 mmol) and triethylamine (685 μL, 4.87 mmol) in acetonitrile (10 mL) is stirred at room temperature over night. Water ist added, and the mixture is extracted with dichloromethane. The phases are separated, and the organic layer is concentrated under reduced pressure. The residue is by purified by preparative HPLC (Waters it) Xbridge™-C18, gradient of acetonitrile in water, 0.1% TFA). Yield: 364 mg; ESI mass spectrum [M+H]+=426; Retention time HPLC: 0.65 min (X012_S01).

1. extractionthe mixture is extracted with dichloromethane
2. customThe phases are separated
3. concentrationthe organic layer is concentrated under reduced pressure
4. customby purified by preparative HPLC (Waters it) Xbridge™-C18, gradient of acetonitrile in water, 0.1% TFA)
5. custom0.65 min (X012_S01)