Hydroxylamine → HCID 86751692, compound

HRID 1938766Notes

Reaction equation

HRID 1938766 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 pressure 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 pressure

Sources & evidence

ORD record
ord-1aaa49f37bf349baab54a9e4cb99a422
Source dataset
uspto-grants-1997_12
Patent number
US05693636

Reaction notes

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