Methylamine → 4-(Methylamino)-3-nitrophenyl phenyl ketone

HRID 2058021

Reaktionsgleichung

Reaktionsgleichung von HRID 2058021
Cl[C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][C:3]=1[N+:16]([O-:18])=[O:17].[CH3:19][NH2:20].S1(CCCC1)(=O)=O>CO>[CH3:19][NH:20][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][C:3]=1[N+:16]([O-:18])=[O:17]

Komponenten

5

Edukt 3

HCID 6329MethylamineHCID 31347SulfolaneHCID 417434-Chloro-3-nitrobenzophenone

Produkt 1

HCID 966894-(Methylamino)-3-nitrophenyl phenyl ketone

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

11 g of 4-chloro-3-nitro-benzophenone, 20 g of methylamine, 153.4 g of methanol and 27.5 g of sulpholane are warmed to 125° for 15 hours in a closed vessel. The reaction solution is evaporated to dryness, the residue is boiled thoroughly with 400 ml of 2 N hydrochloric acid for 20 minutes and the precipitate is filtered off, washed with water and dissolved in methylene chloride. After drying over sodium sulphate and evaporating, 4-methylamino-3-nitro-benzophenone with a melting point of 198°-201° is obtained.

Aufarbeitung

  1. customThe reaction solution is evaporated to dryness
  2. filtrationthe precipitate is filtered off
  3. washwashed with water
  4. dissolutiondissolved in methylene chloride
  5. dry with materialAfter drying over sodium sulphate
  6. customevaporating

Quellen und Nachweise

ORD-Eintrag
ord-ace2d1fe7e91416598de2d7587d90002
Quelldatensatz
uspto-grants-1980_07
Patentnummer
US04213993

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