反应详情

To a solution of 2-methoxy-6-methylphenylamine (8.23 g, 60 mmol) in a mixture of water (60 ml) and tert-butyl methyl ether (60 ml) was added, successively 2-iodononafluorobutane (24.9 g, 11.86 ml, 72 mmol), sodium hydrosulfite (15.29 g, 72 mmol), sodium hydrogen carbonate (6.05 g, 72.0 mmol) and tetrabutyl ammonium hydrogen sulfate (“TBAHS”) (2.24 g, 6.60 mmol). The reaction mixture was stirred at ambient temperature for 16 hours. The mixture was filtered and the filtrate was extracted twice with tert-butyl methyl ether. The combined organic phases were washed with aqueous hydrochloric acid (1N), dried over sodium sulfate and concentrated to give 4-(1,2,2,3,3,3-hexafluoro-1-trifluoromethylpropyl)-2-methoxy-6-methylphenylamine which was used without further purification. LC-MS (Method 2): RT=2.05, [M+H]+=356.

1. additionwas added
2. filtrationThe mixture was filtered
3. extractionthe filtrate was extracted twice with tert-butyl methyl ether
4. washThe combined organic phases were washed with aqueous hydrochloric acid (1N)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated