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Methyl iodide → 2-(Methylamino)-4-nitrophenol

HRID 1585098
Notes
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Reaction equation

HRID 1585098 reaction equation
C([N:3]([CH2:6]C)[CH2:4][CH3:5])C.NC1C=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[CH:11][C:10]=1[OH:18].CI>CO>[CH3:6][NH:3][C:4]1[CH:5]=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[CH:11][C:10]=1[OH:18]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6328Methyl iodide2×HCID 8471Triethylamine2×HCID 36133892-Amino-4-Nitrophenol

Product 1

HCID 212217592-(Methylamino)-4-nitrophenol

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
40 °C

Procedure

Triethylamine (2 ml, 14.4 mmol) was added to a solution of 2-amino-4-nitrophenol (1) (1.54 g, 10 mmol) and methyl iodide (1 ml, 16 mmol) in methanol (10 ml). After 1 hour at 40° C., further methyl iodide (1 ml) and triethylamine (1 ml) were added and the mixture was stirred at 40° C. for a further 2 hours. The reaction mixture was concentrated to dryness in vacuo, the residue was added to aqueous 2N sodium acetate solution and the mixture was extracted with ethyl acetate. The organic phase was dried with sodium sulfate and chromatographed on silica gel (eluent dichloromethane/methanol 95/5). Yield 880 mg (52%).

Workup

  1. concentrationThe reaction mixture was concentrated to dryness in vacuo
  2. additionthe residue was added to aqueous 2N sodium acetate solution
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe organic phase was dried with sodium sulfate
  5. customchromatographed on silica gel (eluent dichloromethane/methanol 95/5)

Sources & evidence

ORD record
ord-66aae1aa20a84164b9801f127695ea82
Source dataset
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05935995

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes