反应详情

温度

45 °C

Sulphuric acid solution (2N,169 ml) was diluted with water (106 ml) and added rapidly dropwise to a stirred solution of 3-[2-(dimethylamino)ethyl]-N-methyl-1H-indole-5-methanesulphonamide (100 g) in ethanol (2.3 l) and water (25 ml) at reflux. The resulting solution was cooled to 45° C.; then seeded, cooled to 4° C. and aged 1 h. The reaction mixture was filtered and the filtrate washed with ethanol (50 ml) then dried at 40° C. in vacuo to give the title compound (114 g) in a solvated form, m.p. 157° C. (decomp.).

1. temperatureat reflux
2. temperaturecooled to 4° C. and aged 1 h
3. filtrationThe reaction mixture was filtered
4. washthe filtrate washed with ethanol (50 ml)
5. customthen dried at 40° C. in vacuo