Hydroxylamine → HCID 86751692, compound

HRID 365641Notes

Reaction equation

HRID 365641 reaction equation
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][CH2:10][C:11]2=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].[NH2:15][OH:16].C([O-])(=O)C.[Na+]>CO>[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([CH2:8][CH2:9][C:10](=[N:15][OH:16])[CH2:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2]

Participants

5

Reactant 3

HCID 787HydroxylamineHCID 384457-Nitro-1-tetraloneHCID 517045Sodium Acetate

Product 1

HCID 86751692HCID 86751692, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 7-nitrotetralone (4.20 g, 22.0 mmol) in methanol (100 mL) was cooled to 0° C., and hydroxylamine (1.68 g, 23.2 mmol) and sodium acetate (3.69 g, 46.4 mmol) were added. The reaction was then stirred at room temperature for 12 h. The methanol was evaporated at reduced pressure and dichloromethane (100 mL) was added. The mixture was washed with water, dried over NaSO4 and evaporated at reduced presure to yield the title compound (4.37 g, 97%). MS (DCI/NH3) m/e 207 [M+H]+.

Workup

  1. customThe methanol was evaporated at reduced pressure and dichloromethane (100 mL)
  2. additionwas added
  3. washThe mixture was washed with water
  4. dry with materialdried over NaSO4
  5. customevaporated at reduced presure

Sources & evidence

ORD record
ord-7e8b81cbb83d46d1a4150ff80c5aaea7
Source dataset
uspto-grants-2000_10
Patent number
US06127359

Reaction notes

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