反应详情

2-Chlorobenzenesulfonyl chloride (92.4 mg, 0.44 mmol) was added to a solution of 3-(4-Amino-butyl)-7,8-dimethoxy-2a,3,4,5-tetrahydro-2H-3-aza-acenaphthylen-1-one dihydro-chloride (150 mg, 0.40 mmol) and NN′-diisopropylethylamine (0.400 ml) in CH2Cl2 (20 mL) and the mixture was stirred overnight at room temperature. The resulting solution was washed with water (3×20 mL), dried over Na2SO4 and evaporated to dryness. The free base was dissolved in ethyl acetate (2 ml) and A 2.8 M solution of hydrogen chloride in ethanol was then added. The product was crystallized and collected by filtration, and vacuum dried to give a pale brown solid (135 mg, 66%).

1. washThe resulting solution was washed with water (3×20 mL)
2. dry with materialdried over Na2SO4
3. customevaporated to dryness
4. dissolutionThe free base was dissolved in ethyl acetate (2 ml)
5. additionA 2.8 M solution of hydrogen chloride in ethanol was then added
6. customThe product was crystallized
7. filtrationcollected by filtration, and vacuum
8. customdried