反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
To a suspension of 2-ethyl-6-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenylamine (0.082 g, 0.27 mmol) (prepared according to EP 1,006,102) and finely ground potassium carbonate (0.112 g, 0.81 mmol) in deuterochloroform (1.0 ml) under stirring at 25° C., was added 3-sulfinylamino-benzoyl chloride (0.055 g, 0.27 mmol) (Example 1.1) dissolved in dry deuterochloroform (1.0 ml). The reaction mixture was stirred at 40° C. for 16 hours. A sample of the supernatant 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. 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: 467.00.
WORKUP
后处理
- stirringThe reaction mixture was stirred at 40° C. for 16 hours