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

HRID 1391351

Reaction equation

HRID 1391351 reaction equation
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]

Participants

5

Reactant 3

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

Product 1

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

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-304054e680f44aa9bc84df41663b746a
Source dataset
uspto-grants-1979_02
Patent number
US04141982

Linked notes

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