Methanol → HCID 21556923, Verbindung

HRID 267331

Reaktionsgleichung

Reaktionsgleichung von HRID 267331
[CH3:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][C:5]([N+:11]([O-:13])=[O:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].Cl[C:18]1[C:19]([N+:45]([O-:47])=[O:46])=[C:20]([C:30]2[C:35]([N+:36]([O-:38])=[O:37])=[CH:34][C:33]([N+:39]([O-:41])=[O:40])=[CH:32][C:31]=2[N+:42]([O-:44])=[O:43])[C:21]([N+:27]([O-:29])=[O:28])=[CH:22][C:23]=1[N+:24]([O-:26])=[O:25].CO>CC(C)=O>[N+:8]([C:7]1[CH:6]=[C:5]([N+:11]([O-:13])=[O:12])[CH:4]=[C:3]([N+:14]([O-:16])=[O:15])[C:2]=1[CH2:1][C:22]1[C:21]([N+:27]([O-:29])=[O:28])=[C:20]([C:30]2[C:31]([N+:42]([O-:44])=[O:43])=[CH:32][C:33]([N+:39]([O-:41])=[O:40])=[CH:34][C:35]=2[N+:36]([O-:38])=[O:37])[C:19]([N+:45]([O-:47])=[O:46])=[CH:18][C:23]=1[N+:24]([O-:26])=[O:25])([O-:10])=[O:9]

Komponenten

5

Edukt 3

HCID 887MethanolHCID 83762,4,6-TrinitrotolueneHCID 14927170HCID 14927170, Verbindung

Produkt 1

HCID 21556923HCID 21556923, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

The reaction of 4.5 g (0.02 mole) of TNT with 4.6 g, (0.01 mole) of 3-chloro-2,2',4,4',6,6'-hexanitrobiphenyl was carried out as above. After extracting the crude reaction product with methanol until the extracts were light colored, the somewhat gummy residue was dissolved in acetone, an equal volume of methanol was added and the solution was heated, with magnetic stirring, on a hot plate. A light yellow crystalline material separated, was filtered off and dried. It weighed 1.7 g, 25% of the theoretical yield. Recrystallized from acetone methanol formed faintly yellow rod-like crystals, mp 255°-256°. Anal. Calcd for C19H7N9O18 : C, 35.1; H, 1.1; N, 19.4. Found: C, 34.9, 34.2; H, 1.6, 1.2; N, 19.2, 18.8.

Aufarbeitung

  1. extractionAfter extracting the crude
  2. customreaction product with methanol until the extracts
  3. temperaturethe solution was heated, with magnetic stirring, on a hot plate
  4. customA light yellow crystalline material separated
  5. filtrationwas filtered off
  6. customdried
  7. customRecrystallized from acetone methanol
  8. customformed faintly yellow rod-like crystals, mp 255°-256°

Quellen und Nachweise

ORD-Eintrag
ord-8d32c2f24e7b4d6f9293d7a817d07d8f
Quelldatensatz
uspto-grants-1976_03
Patentnummer
US03941853

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