Hydroxyamine hydrochloride → HCID 3729139, compound

HRID 508506Notes

Reaction equation

HRID 508506 reaction equation
C([O-])(=O)C.[Na+].Cl.[NH2:7][OH:8].[C:9]1(=O)[CH:12]2[CH2:13][C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=3[CH:11]2[CH2:10]1>CO>[C:9]1(=[N:7][OH:8])[CH:12]2[CH2:13][C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=3[CH:11]2[CH2:10]1

Participants

5

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 126384102,2a,7,7a-Tetrahydro-1H-cyclobuta[a]inden-1-one

Product 1

HCID 3729139HCID 3729139, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Sodium acetate (1.45 g, 17.7 mmol) and hydroxylamine hydrochloride (0.68 g, 9.75 mmol) were added to a solution of 2,2a,7,7a-tetrahydro-cyclobuta[a]inden-1-one (1.4 g, 8.86 mmol) in MeOH (18 mL), and stirred overnight at room temperature. The reaction solution was concentrated via rotary evaporation. The residue was dissolved in CH2Cl2 (100 mL), washed with H2O (50 mL), dried over MgSO4, and concentrated to give the subtitle compound, which was used without further purification. MS calculated for C11H11NO+H: 174, observed: 174.

Workup

  1. concentrationThe reaction solution was concentrated via rotary evaporation
  2. dissolutionThe residue was dissolved in CH2Cl2 (100 mL)
  3. washwashed with H2O (50 mL)
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated

Sources & evidence

ORD record
ord-c336606baa6b46f5985a60196cff41b0
Source dataset
uspto-grants-2015_08
Patent number
US09096520B2

Reaction notes

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