Methane → Benzenamine, 3-chloro-2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)-

HRID 1658946

Reaktionsgleichung

Reaktionsgleichung von HRID 1658946
[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].[CH2:19]([NH:22][CH2:23][CH2:24][CH3:25])[CH2:20][CH3:21].C>C(O)C>[CH2:19]([N:22]([CH2:23][CH2:24][CH3:25])[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])[CH2:20][CH3:21]

Komponenten

5

Edukt 3

HCID 297MethaneHCID 8902DipropylamineHCID 943982,4-Dichloro-1,3-dinitro-5-(trifluoromethyl)benzene

Produkt 1

HCID 94399Benzenamine, 3-chloro-2,6-dinitro-N,N-dipropyl-4-(trifluoromethyl)-Ausbeute 79,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

A heavy walled glass reaction tube of approximately 50 ml. capacity was charged with 7.0 grams (0.023 mole) of 2,4-dichloro-3,5-dinitrobenzotrifluoride, 4.64 grams (0.0458 mole) of di-n-propylamine and 40 ml. of absolute ethanol. The tube was sealed and heated in an oil bath at 94°-99°C. for 98 hours. The cooled reaction mixture was then evaporated to dryness to give an oily residue which was extracted with boiling diethyl ether. The insoluble di-n-propylamine hydrochloride was removed by filtration and washed with additional ether. The combined ether filtrates were evaporated to give an oily orange residue which was dissolved in 100 ml. of absolute ethanol and decolorized with activated charcoal. The ethanol and volatiles were removed by evaporation under reduced pressure to give the product (6.77 grams) as a viscous reddish oil.

Aufarbeitung

  1. customA heavy walled glass reaction tube of approximately 50 ml
  2. customThe tube was sealed
  3. temperatureheated in an oil bath at 94°-99°C. for 98 hours
  4. customThe cooled reaction mixture
  5. customwas then evaporated to dryness
  6. customto give an oily residue which
  7. extractionwas extracted with boiling diethyl ether
  8. customThe insoluble di-n-propylamine hydrochloride was removed by filtration
  9. washwashed with additional ether
  10. customThe combined ether filtrates were evaporated
  11. customto give an oily orange residue which
  12. dissolutionwas dissolved in 100 ml
  13. customThe ethanol and volatiles were removed by evaporation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cb7ca2022d994848beb0fefa0503376b
Quelldatensatz
uspto-grants-1976_06
Patentnummer
US03966816

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