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Hydroxyamine hydrochloride → HCID 76688560, compound

HRID 2096974
Notes
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Reaction equation

HRID 2096974 reaction equation
Cl.[NH2:2][OH:3].[F:4][C:5]1[C:12]([I:13])=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=O>C(O)C>[F:4][C:5]1[C:12]([I:13])=[CH:11][CH:10]=[CH:9][C:6]=1[CH:7]=[N:2][OH:3]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 227141892-Fluoro-3-iodobenzaldehyde

Product 1

HCID 76688560HCID 76688560, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A 50% aqueous solution of hydroxylamine hydrochloride (9 mL, 64.8 mmol) was added to a stirred suspension of 2-fluoro-3-iodobenzaldehyde (preparation 22d, 2.10 g, 8.4 mmol) in ethanol (10 mL) and the mixture was warmed slightly until a solution was formed. After stirring for 3 days at room temperature, the mixture was concentrated in vacuo and water was added to the residue. The mixture was extracted with ethyl acetate and the organic layer was washed with brine, dried (MgSO4) and evaporated to give the title compound (2.15 g, 97%) as a solid.

Workup

  1. temperaturethe mixture was warmed slightly until a solution
  2. customwas formed
  3. concentrationthe mixture was concentrated in vacuo and water
  4. additionwas added to the residue
  5. extractionThe mixture was extracted with ethyl acetate
  6. washthe organic layer was washed with brine
  7. dry with materialdried (MgSO4)
  8. customevaporated

Sources & evidence

ORD record
ord-43a87c5b3b494852bb33b22d56ad74b3
Source dataset
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08450341B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes