反应详情

温度

50 °C

A suspension of 3-amino-N-[2-ethyl-6-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-benzamide (0.100 g, 0.237 mmol) (Example 4.1) in carbon tetrachloride (1 ml) was heated to 50° C. until it became a clear solution. A solution of thionyl chloride in carbon tetrachloride (1.68 M) (0.725 ml, 1.218 mmol) was added and the mixture was heated to 80° C. for one hour. The reaction mixture was evaporated under reduced pressure and the residue was triturated with cyclohexane. The suspension was filtered and the solid dried under high vacuum. The desired compound was obtained as white crystals. M.p. 100-108° C. 1H-NMR as described for Example 2.2. Mass spectrometric analysis: conditions as described for Example 2.1. Calculated exact mass: 468; [M-H]− observed: 467.06.

1. temperaturethe mixture was heated to 80° C. for one hour
2. customThe reaction mixture was evaporated under reduced pressure
3. customthe residue was triturated with cyclohexane
4. filtrationThe suspension was filtered
5. customthe solid dried under high vacuum