反应详情

温度

0 °C

A stirred mixture of 3.82 g (0.02 mol) of 5,6-dimethoxy-2-methylindole and 5,80 g (0.044 mol) of potassium carbonate in 50 ml. of chloroform and 15 ml. of water is cooled to -5° C. Then 3.2 g (0.024 mol) of oxalyl chloride is added slowly, maintaining the reaction temperature at 0° C. The resulting mixture is stirred at room temperature for 10 minutes. Then 3.5 g (0.03 mol) of nitrosopiperazine is added over a 5 minute span. The reaction mixture turns red-purple and is stirred for an additional hour. To the solution is slowly added in portions 250 ml. of ethyl ether; the solution appears lighter and a tan precipitate forms. After stirring for one hour, the product is filtered, washed well with water and dried. This product is recrystallized from a DMF and water mixture to give flakes of 1-(5,6-dimethoxy-2-methylindol-3-ylglyoxyloyl)-4-nitrosopiperazine, m.p. 233°-225° C. Analysis: Calculated for C17H20N4O5 : 56.66% C; 5.59% H; 15.55% N Found: 56.65% C; 5.61% H; 15.68% N.

1. stirringis stirred for an additional hour
2. additionTo the solution is slowly added in portions 250 ml
3. stirringAfter stirring for one hour
4. filtrationthe product is filtered
5. washwashed well with water
6. customdried
7. customThis product is recrystallized from a DMF and water mixture