1,1-Dimethylhydrazine → N-dimethylamino-3-chloro-2,6-dinitro-4-trifluoromethylaniline

HRID 1390171Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1390171
[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6](Cl)[C:5]([N+:12]([O-:14])=[O:13])=[CH:4][C:3]=1[C:15]([F:18])([F:17])[F:16].[CH3:19][N:20]([CH3:22])[NH2:21]>C1CCCCC1>[CH3:19][N:20]([CH3:22])[NH:21][C:6]1[C:5]([N+:12]([O-:14])=[O:13])=[CH:4][C:3]([C:15]([F:18])([F:17])[F:16])=[C:2]([Cl:1])[C:7]=1[N+:8]([O-:10])=[O:9]

Komponenten

4

Edukt 2

HCID 59761,1-DimethylhydrazineHCID 943982,4-Dichloro-1,3-dinitro-5-(trifluoromethyl)benzene

Produkt 1

HCID 13101276N-dimethylamino-3-chloro-2,6-dinitro-4-trifluoromethylanilineAusbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8078CyclohexaneLösungsmittel

Versuchsvorschrift

To 20.0 g. (0.065 mole) of 2,4-dichloro-3,5-dinitrobenzotrifluoride and 300 ml. of cyclohexane in a 500 ml. roundbottom flask equipped with a stirrer and dropping funnel was added 7.86 g. (0.13 mole) of 1,1-dimethylhydrazine at ambient temperature. The addition was drop-wise over a period of about 20 minutes. Stirring was continued for 22 hours at room temperature. The resultant mixture was filtered and the insoluble solid then stirred with 300 ml. of water for one hour to dissolve the hydrazine hydrochloride. The insoluble product was isolated by filtration and washed with water. Recrystallization from 95% ethanol gave 18.3 g. (85%) of the desired product as a yellow solid, m.p. 130° - 131° C.

Aufarbeitung

  1. customroundbottom flask equipped with a stirrer
  2. additionwas added 7.86 g
  3. customat ambient temperature
  4. additionThe addition
  5. waitwas continued for 22 hours at room temperature
  6. filtrationThe resultant mixture was filtered
  7. stirringthe insoluble solid then stirred with 300 ml
  8. dissolutionof water for one hour to dissolve the hydrazine hydrochloride
  9. customThe insoluble product was isolated by filtration
  10. washwashed with water
  11. customRecrystallization from 95% ethanol
  12. customgave 18.3 g

Quellen und Nachweise

ORD-Eintrag
ord-0129388f688e4c64a9074135c36c8b99
Quelldatensatz
uspto-grants-1979_02
Patentnummer
US04138244

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