反应详情

温度

25 °C

5-(4-Methylpiperazine-1-ylmethyl)-1H-indole (0.8733 mmol, 0.2 gram) (obtained from Example 1) was dissolved in 2 mL N,N-dimethyl formamide. The above solution was then added slowly to 25 mL flask, containing a suspension of sodium hydride (1.31 mmol, 31.4 mg) in 1 mL DMF under nitrogen atmosphere, while maintaining the temperature below 10° C. The reaction mixture was then stirred for a period of 1 hour at 25° C. To this well stirred solution, benzenesulfonyl chloride (1.31 mmol, 0.2312 gram) was added slowly while maintaining the temperature below 10° C. The reaction mixture was further stirred for a period of 2 hours. After the completion of the reaction, the reaction mixture was poured onto 20 grams of ice-water mixture under stirring and the resulting mixture was extracted with ethyl acetate (2×20 mL). The combined ethyl acetate extracts were then washed with water (20 mL), brine (20 mL) and dried over anhydrous sodium sulfate. The volatiles were removed under the reduced pressure to obtain thick syrupy mass, which was purified over silica gel column, eluent being ethyl acetate and triethylamine (0.2 to 1.0%). This material was converted to dihydrochloride salt in diethylether solvent.

1. additionThe above solution was then added slowly to 25 mL flask
2. additioncontaining
3. temperaturewhile maintaining the temperature below 10° C
4. temperaturewhile maintaining the temperature below 10° C
5. stirringThe reaction mixture was further stirred for a period of 2 hours
6. customAfter the completion of the reaction
7. stirringunder stirring
8. extractionthe resulting mixture was extracted with ethyl acetate (2×20 mL)
9. washThe combined ethyl acetate extracts were then washed with water (20 mL), brine (20 mL)
10. dry with materialdried over anhydrous sodium sulfate
11. customThe volatiles were removed under the reduced pressure
12. customto obtain thick syrupy mass, which
13. customwas purified over silica gel column, eluent