1-Methylpiperazine → 5-[(4-Methyl-1-piperazinyl)-carbonyl]-6,7-dibromo-8-nitro-1,4-benzodioxane
Reaktionsgleichung
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[Br:8][C:9]1[C:18]([Br:19])=[C:17]([N+:20]([O-:22])=[O:21])[C:12]2[O:13][CH2:14][CH2:15][O:16][C:11]=2[C:10]=1[C:23](Cl)=[O:24]>>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:23]([C:10]2[C:11]3[O:16][CH2:15][CH2:14][O:13][C:12]=3[C:17]([N+:20]([O-:22])=[O:21])=[C:18]([Br:19])[C:9]=2[Br:8])=[O:24])[CH2:4][CH2:3]1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 10 °C
Versuchsvorschrift
400 ml of methylethylcetone 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%).
Aufarbeitung
- customprovided with an agitator
- temperaturebeing maintained below 20° C
- customAfter agitation of the mixture, the crystals were dried off
- washwashed with methylethylcetone
- customdried
- dissolutiondissolved in water
- customreprecipitated by addition of 50 ml of 20% ammonia
- customThe crystals were dried off
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-9d97006e7fa448349ce0928c6b49d58c
- Quelldatensatz
- uspto-grants-1981_12
- Patentnummer
- US04306072
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