反应详情

温度

100 °C

To a solution of 5,6-dimethoxy-2-aminoindan (Preparation 5, 4.5 mmol) in dimethylformamide/acetonitrile (1:6, 49 mL) was added sodium carbonate (1.43 g, 13.5 mmol) and was heated (100° C.) overnight. The mixture was diluted with ethyl acetate, filtered and the filtrate concentrated. The oily residue was chromatographed (400 g silica gel) eluting with methylene chloride/methanol (9:1) to yield a yellow oil. The oil was converted into the HCl salt and recrystallized from methanol/ethyl acetate: mp 267°-269° C.

1. filtrationfiltered
2. concentrationthe filtrate concentrated
3. customThe oily residue was chromatographed (400 g silica gel)
4. washeluting with methylene chloride/methanol (9:1)
5. customto yield a yellow oil
6. customrecrystallized from methanol/ethyl acetate