Water → N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamide

HRID 2052668

Reaktionsgleichung

Reaktionsgleichung von HRID 2052668
[NH2:1][N:2]1[CH2:7][CH2:6][N:5]([CH3:8])[CH2:4][CH2:3]1.[N+:9]([C:12]1[CH:13]=[C:14]([C:22](Cl)=[O:23])[C:15]2[O:20][CH2:19][CH2:18][O:17][C:16]=2[CH:21]=1)([O-:11])=[O:10].O>C(C(C)=O)C>[CH3:8][N:5]1[CH2:6][CH2:7][N:2]([NH:1][C:22]([C:14]2[C:15]3[O:20][CH2:19][CH2:18][O:17][C:16]=3[CH:21]=[C:12]([N+:9]([O-:11])=[O:10])[CH:13]=2)=[O:23])[CH2:3][CH2:4]1

Komponenten

5

Edukt 3

HCID 962WaterHCID 813491-Amino-4-methylpiperazineHCID 205447457-Nitro-1,4-benzodioxane-5-carbonyl chloride

Produkt 1

HCID 20544699N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamideAusbeute 55,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6569Methyl Ethyl KetoneLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

33 g of 1-amino-4-methylpiperazine were dissolved in 630 ml of methyl ethyl ketone. The mixture was cooled to 10° C. and 61 g of 7-nitro-1,4-benzodioxane-5-carbonyl chloride were introduced by portions. The mixture was stirred for two hours and then the solid was filtered off and washed with 150 ml of methyl ethyl ketone. The obtained product was purified by transformation into the base (M.P.: 212° C.) and recrystallized by treatment with hydrochloric ethanol. 45 g of N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamide were obtained (M.P.: 210° C. with one mole of water). The structure was confirmed by nuclear magnetic resonance and infrared analyses.

Aufarbeitung

  1. filtrationthe solid was filtered off
  2. washwashed with 150 ml of methyl ethyl ketone
  3. customThe obtained product was purified by transformation into the base (M.P.: 212° C.)
  4. customrecrystallized by treatment with hydrochloric ethanol

Quellen und Nachweise

ORD-Eintrag
ord-0d6b2e8bffc641e787a5d73eca06e669
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04186135

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