反应详情

温度

25 °C

To a solution of 2-ethyl-6-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenylamine (0.100 g, 0.33 mmol) (prepared according to EP 1,006,102) in deuterochloroform (1.0 ml) was added under stirring at 25° C., a solution of 3-sulfinylamino-benzoyl chloride (0.033 g, 0.165 mmol) (Example 1.1) in dry deuterochloroform (1.0 ml). After stirring for 8 hours at 40° C., a sample of the reaction mixture was submitted to 1H-NMR spectroscopy. The desired compound was detected in the reaction mixture, based on its characteristic signals (see 1H-NMR spectral data as described in Example 2.2), together with unreacted starting materials. Integration of the signals showed a conversion of 85%. An aliquot of the reaction mixture was diluted in dry acetonitrile and was submitted to mass spectrometry via direct injection (same conditions as described in Example 2.1). Calculated exact mass: 468; [M-H]− observed: 467.06.

1. stirringAfter stirring for 8 hours at 40° C.