反应详情

To a solution of 2.1 g (10 mmole) of 2-{N-(2-aminoethyl)]aminomethyl-2,3-dihydrobenzodioxin and 1.3 g (10 mmole) of diisopropylethylamine in 100 ml of dichloromethane stored in an ice bath was added 1.8 g (7.2 mmole) (-)-10-camphorsulfonyl chloride. The mixture was allowed to stir overnight at room temperature. The reaction was next washed with saturated aqueous sodium bicarbonate, with saturated sodium chloride, dried over sodium sulfate, filtered and evaporated in vacuum. Column chromatography on 100 g of silica gel with chloroform as eluant, followed by crystallization from isopropanol gave 1.3 g of the title compound, m.p. 149°-152° C.

1. washThe reaction was next washed with saturated aqueous sodium bicarbonate, with saturated sodium chloride
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. customevaporated in vacuum
5. customColumn chromatography on 100 g of silica gel with chloroform as eluant, followed by crystallization from isopropanol