反应详情

温度

-5 °C

To a stirred mixture of 9.0 g of lithium aluminum hydride in 400 ml. of 1,2-dimethoxyethane is added 10.52 g (0.35 mol) of 1-(2-methylindol-3-ylglyoxyloyl)-4-nitrosopiperazine slowly to maintain reaction temperature below 35° C. After all the material is added, the mixture is refluxed for 14-16 hours. The reaction mixture is cooled to -5° C. and a solution of 50 ml. of water and 50 ml. of 1,2-dimethoxyethane is slowly added while maintaining the temperature below 15° C. Another 50 ml. of water is added. The mixture is then filtered, the solvent is removed, and the residual solid is recrystallized from hot benzene, producing the pure crystals of 3-[2-(4-aminopiperazin-1-yl)ethyl]-2-methylindole, m.p. 118°-120° C. Analysis: Calculated for C15H22N4 : 71.08% C; 8.21% H; 20.72% N Found:71.11% C; 8.28% H; 20.75 % N.

1. temperatureto maintain
2. customreaction temperature below 35° C
3. additionAfter all the material is added
4. temperaturethe mixture is refluxed for 14-16 hours
5. temperaturewhile maintaining the temperature below 15° C
6. filtrationThe mixture is then filtered
7. customthe solvent is removed
8. customthe residual solid is recrystallized from hot benzene