Reaktion #214616

Reaktionsgleichung

methylpiperazine

6,7-dibromo-8-nitro-1,4-benzodioxane-5-carbonyl chloride

→

5-[(4-methyl-1-piperazinyl)-carbonyl]-6,7-dibromo-8-nitro-1,4-benzodioxane

Ausbeute 69.6%

Lösungsmittel

methylethylacetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprovided with an agitator
2. 2
   Temperaturbeing maintained below 20° C
3. 3
   SonstigeAfter agitation of the mixture, the crystals were dried off
4. 4
   Waschenwashed with methylethylcetone
5. 5
   Sonstigedried
6. 6
   workup.DISSOLUTIONdissolved in water
7. 7
   Sonstigereprecipitated by addition of 50 ml of 20% ammonia
8. 8
   SonstigeThe crystals were dried off
9. 9
   Waschenwashed with water
10. 10
    Sonstigedried

Vorschrift

400 ml of methylethylacetone and 11 g of methylpiperazine were introduced into a balloon flask provided with an agitator and a thermometer. The mixture was cooled to 10° C. and then 41 g of 6,7-dibromo-8-nitro-1,4-benzodioxane-5-carbonyl chloride were added in portions with the temperature being maintained below 20° C. After agitation of the mixture, the crystals were dried off, washed with methylethylcetone and dried and then dissolved in water and reprecipitated by addition of 50 ml of 20% ammonia. The crystals were dried off, washed with water and dried. 33 g of 5-[(4-methyl-1-piperazinyl)-carbonyl]-6,7-dibromo-8-nitro-1,4-benzodioxane were obtained (M.P: 164° C.; yield: 69.6%).

Quelle