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Potassium Hydroxide → 4-Amino-N-hydroxy-2-methoxybenzamide

HRID 1096577
Notes
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Reaction equation

HRID 1096577 reaction equation
[CH3:1][O:2][C:3]1[CH:12]=[C:11]([NH2:13])[CH:10]=[CH:9][C:4]=1[C:5](OC)=[O:6].Cl.[NH2:15][OH:16].[OH-].[K+]>CO>[NH2:13][C:11]1[CH:10]=[CH:9][C:4]([C:5]([NH:15][OH:16])=[O:6])=[C:3]([O:2][CH3:1])[CH:12]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 14797Potassium HydroxideHCID 168705Methyl 4-amino-o-anisateHCID 443297Hydroxyamine hydrochloride

Product 1

HCID 160422934-Amino-N-hydroxy-2-methoxybenzamideYield 47%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

Methyl 2-methoxy-4-aminobenzoate (10 g, 55.25 mmol) and hydroxylamine hydrochloride (15.36 g, 221 mmol) were taken up in MeOH (80 ml) and a solution of KOH (15.4 g, 275 mmol) in MeOH (55 ml) was added carefully. The resultant mixture was stirred at reflux for 36 hrs. The volatiles were removed in vacuo. The residue was taken up in 1M NaOH (50 ml) and washed with ethyl acetate (EtOAc, 50 ml). Concentrated HCl was added slowly until precipitation of a solid (pH was 10). The solid was filtered off, washed with H2O, then methyl-tert-butyl ether (MTBE) and dried under vacuum. 1H NMR showed the solid contained approx. 1/3 molar equivalent of ethyl acetate. The solid was taken up in 1M NaOH (100 ml) and the EtOAc was removed in vacuo. Concentrated HCl was added carefully until precipitation of a solid (pH was 8). The solid was collected by filtration, washed with H2O, then MTBE and dried under vacuum to give 4.67 g (47%) of the title compound as a dark red solid.

Workup

  1. temperatureat reflux for 36 hrs
  2. customThe volatiles were removed in vacuo
  3. washwashed with ethyl acetate (EtOAc, 50 ml)
  4. additionConcentrated HCl was added slowly until precipitation of a solid (pH was 10)
  5. filtrationThe solid was filtered off
  6. washwashed with H2O
  7. dry with materialmethyl-tert-butyl ether (MTBE) and dried under vacuum
  8. customthe EtOAc was removed in vacuo
  9. additionConcentrated HCl was added carefully until precipitation of a solid (pH was 8)
  10. filtrationThe solid was collected by filtration
  11. washwashed with H2O
  12. dry with materialMTBE and dried under vacuum

Sources & evidence

ORD record
ord-bdd1851377004985bdae0e38546a48f1
Source dataset
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08138357B2

Reaction notes

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