反应详情

To a stirred solution of 1.5 g of (+) three 1-phenoxymethyl-1-(4-benzylpiperidin-1-yl)-2-p-aminophenyl-2-hydroxy-ethane and 1.43 g of KSCN in 20 ml of glacial acetic acid was added dropwise a solution of 0.58 g of Br2 in 5 ml of glacial acetic acid at room temperature. After stirring for 2 h., the yellow sospension was filtered and the solution was poured into 70 ml of concentrated ammonium solution. The cloudy basic solution was extracted with ethyl acetate dried and evaporated. The resulting yellow residue was chromatographed on silica gel eluting with ethylacetate/cycloexane ⅓, furnishing after crystallization from ethanol 0.9 g of the title compound, m.p. 210-214° C., [α]20D=−2.1±0.1

1. filtrationthe yellow sospension was filtered
2. additionthe solution was poured into 70 ml of concentrated ammonium solution
3. extractionThe cloudy basic solution was extracted with ethyl acetate
4. customdried
5. customevaporated
6. customThe resulting yellow residue was chromatographed on silica gel eluting with ethylacetate/cycloexane ⅓
7. customfurnishing
8. customafter crystallization from ethanol 0.9 g of the title compound, m.p. 210-214° C., [α]20D=−2.1±0.1