反应详情

温度

60 °C

The mixture of 5.4 g (0.033 mol) (-)-2-aminomethylchroman (example 92f; αD =-122.8), 6.1 g (0.06 mol) triethylamine, 9.5 g (0.03 mol) N-(4-bromobutyl) saccharin and 80 ml anhydrous dimethyl formamide was heated to 60° C. for 4 h. The solvent was evaporated at 0.01 torr. The residue (13.5 g) was dissolved in toluene/ethyl acetate (5:1) and chromatographed on silica (300 g). The fraction (5.8 g) obtained by elution with toluene/ethyl acetate 1:1 was rechromatographed on 150 g of silica, providing 3.7 g of chemically pure 2-(N-[4-(1,1-Dioxido-3-oxo-2,3-di-hydro-benzisothiazol-2-yl)butyl]aminomethyl}chroman.

1. customThe solvent was evaporated at 0.01 torr
2. dissolutionThe residue (13.5 g) was dissolved in toluene/ethyl acetate (5:1)
3. customchromatographed on silica (300 g)
4. customThe fraction (5.8 g) obtained by elution with toluene/ethyl acetate 1:1
5. customwas rechromatographed on 150 g of silica