反应详情

To a solution of 3-trifluoroacetyl-9-iodo-1,2,4,5-tetrahydro-3-benzazepine-7-sulfonyl fluoride (5.29, 11.5 mmol) in tetrahydrofuran (50 ml) was added 4-fluorophenylmagnesium chloride (50 ml, 1M in tetrahydrofuran, 50 mmol). The resulting solution was stirred for 18 h without cooling then poured into saturated aqueous sodium potassium tartrate (150 ml), and extracted with diethyl ether (100 ml), The resulting organic layer washed with brine (100 ml), dried (MgSO4), and evaporated. Isolation using an SCX column and crystallisation from diethyl ether gave the subtitle compound as a white solid (2.4 g).

1. temperaturewithout cooling
2. extractionextracted with diethyl ether (100 ml)
3. washThe resulting organic layer washed with brine (100 ml)
4. dry with materialdried (MgSO4)
5. customevaporated
6. customan SCX column and crystallisation from diethyl ether