反应详情

Combine the amine (0.164 g, 0.425 mmol), 3-trifluoromethylphenyl isocyanate (0.060 mL, 0.425 mmol) and triethylamine (0.119 mL, 0.851 mmol) in DMSO (5 mL). Stir the mixture at room temperature for ninety minutes. Extract the mixture with ethyl acetate versus water. Wash the organic layer with saturated aqueous saturated sodium chloride. Dry the resulting organics over magnesium sulfate, filter, and concentrate. Purify by column chromatography (ethyl acetate→5% methanol in dichloromethane→10% methanol in dichloromethane) to afford product (0.056 g, 13%, two steps). MS(ES), m/z 573 (M+1).

1. extractionExtract the mixture with ethyl acetate versus water
2. washWash the organic layer with saturated aqueous saturated sodium chloride
3. dry with materialDry the resulting organics over magnesium sulfate
4. filtrationfilter
5. concentrationconcentrate
6. customPurify by column chromatography (ethyl acetate→5% methanol in dichloromethane→10% methanol in dichloromethane)
7. customto afford product (0.056 g, 13%, two steps)