反应详情

(4-Amino-3-fluorophenyl)(4-(4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)-benzyl)piperazin-1-yl)methanone (0.209 mmol, 0.1 g) and N,N-diisopropylethylamine (0.709 mmol, 0.117 mL, 0.092 g) were stirred in dichloromethane at room temperature. Triphosgene (0.077 mmol, 0.023 g) was added and the reaction mixture stirred for 30 minutes. Isopropylamine (0.417 mmol, 0.036 mL, 0.025 g) was added and the reaction stirred for a further 30 minutes. The reaction was concentrated at reduced pressure and the resulting residue was purified by silica chromatography (eluting with a solvent gradient from dichloromethane to 5% methanol/dichloromethane) to afford the title compound (20 mg). MS (ESI) m/z 565.5 [M+H]+

1. stirringthe reaction stirred for a further 30 minutes
2. concentrationThe reaction was concentrated at reduced pressure
3. customthe resulting residue was purified by silica chromatography (
4. washeluting with a solvent gradient from dichloromethane to 5% methanol/dichloromethane)