Hydroxyamine hydrochloride → HCID 3729139, compound

HRID 1517690Notes

Reaction equation

HRID 1517690 reaction equation
C([O-])(=O)C.[Na+].Cl.[OH:7][NH2:8].[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:8][OH:7])[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 hydroxyl amine 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-4da2f2ba740a46b5858cf302b0b57dfa
Source dataset
uspto-grants-2012_07
Patent number
US08232311B2

Reaction notes

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