Hydroxylamine → HCID 72307495, compound

HRID 219852Notes

Reaction equation

HRID 219852 reaction equation
[C:1]([C:3]1[C:12]([F:13])=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[C:5]([F:14])[CH:4]=1)#[N:2].[NH2:15][OH:16]>CO>[NH2:2][C:1](=[N:15][OH:16])[C:3]1[C:12]([F:13])=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[C:5]([F:14])[CH:4]=1

Participants

4

Reactant 2

HCID 787HydroxylamineHCID 66678474HCID 66678474, compound

Product 1

HCID 72307495HCID 72307495, compoundYield 98.6%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Methyl 4-cyano-2,5-difluorobenzoate (265 mg; 1.34 mmol; 1 eq.) was dissolved in MeOH. Hydroxylamine (0.40 mL; 6.72 mmol; 5 eq.) was added and the mixture was stirred at RT. After one night, the reaction was complete and the solvents were evaporated, affording the title product as a white solid (304 mg; 98%). LC/MS (Method A): 229.0 (M−H)−; 231.0 (M+H)+. HPLC (Method A) Rt 1.08 min (Purity: 98.7%)

Workup

  1. waitAfter one night
  2. customthe solvents were evaporated

Sources & evidence

ORD record
ord-b86e0e08dfa948cda82cf5897c98fada
Source dataset
uspto-grants-2012_06
Patent number
US08202865B2

Reaction notes

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