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 bisulfate (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 bisulfate (100 mL), once with brine (100 mL)
6. dry with materialdried with Na2SO4
7. concentrationconcentrated