反应详情

温度

80 °C

The requisite 1-(5-chloroindol-2-ylsulphonyl)piperazine starting material was prepared as follows 1-(1-Benzenesulphonyl-5-chloroindol-2-ylsulphonyl)piperazine (4.15 g, 9.44 mmol) was treated with sodium hydroxide solution (32 ml of 2.5M), giving a yellow suspension. This was warmed to 80° C. with vigorous stirring and stirred for 45 mins, giving complete solution. The solution was cooled to ambient temperature and carefully treated with concentrated hydrochloric acid to pH 8; the resultant precipitate was filtered off, washed with water and dried to give 1-(5-chloroindol-2-ylsulphonyl)piperazine as a pale yellow solid, 1H NMR (d6DMSO) 2.75 ppm (m, 4H), 2.9 ppm (m, 4H), 7.0 ppm (s, 1H), 7.3 ppm (dd, 1H), 7.5 ppm (d, 1H), 7.8 ppm (d, 1H); MS (M+H)+ 300/302.

1. customThe requisite 1-(5-chloroindol-2-ylsulphonyl)piperazine starting material was prepared
2. customgiving a yellow suspension
3. stirringstirred for 45 mins
4. customgiving complete solution
5. temperatureThe solution was cooled to ambient temperature
6. filtrationthe resultant precipitate was filtered off
7. washwashed with water
8. customdried