反应详情

A solution of N-trifluoroacetyl-1-(3-methoxyphenyl)-2-propylamine (4.29 g, 15.7 mmol) in methanol (100 mL) was cooled to −78 C. and treated with CaCO3 (3.17 g, 31.4 mmol), followed by a solution of ICl (6.37 g, 39.3 mmol) in methanol (50 mL). The reaction was allowed to warm to 20 C. while stirring overnight. The product mixture was filtered, concentrated, dissolved in EtOAc (200 mL), washed twice with 5% aqueous sodium bisulfite (100 mL), once with brine (100 mL), dried with Na2SO4 and concentrated to give 6.72 g of a white solid powder. MS calculated for C12H13F3INO2+H: 388, observed: 388.

1. temperatureto warm to 20 C
2. filtrationThe product mixture was filtered
3. concentrationconcentrated
4. dissolutiondissolved in EtOAc (200 mL)
5. washwashed twice with 5% aqueous sodium bisulfite (100 mL), once with brine (100 mL)
6. dry with materialdried with Na2SO4
7. concentrationconcentrated