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

HRID 1391351

Reaktionsgleichung

Reaktionsgleichung von HRID 1391351
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-304054e680f44aa9bc84df41663b746a
Quelldatensatz
uspto-grants-1979_02
Patentnummer
US04141982

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