Hydroxyamine hydrochloride → HCID 136360171, compound

HRID 2243334Notes

Reaction equation

HRID 2243334 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:9]=[C:8]([C:10]3[C:22]4[C:21]5[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=5)[C:15](=O)[C:14]=4[CH:13]=[CH:12][CH:11]=3)[NH:7][C:6]=2[CH:24]=1.Cl.[NH2:26][OH:27].C([O-])(=O)C.[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:9]=[C:8]([C:10]3[C:22]4[C:21]5[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=5)[C:15](=[N:26][OH:27])[C:14]=4[CH:13]=[CH:12][CH:11]=3)[NH:7][C:6]=2[CH:24]=1

Participants

5

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 67360611HCID 67360611, compound

Product 1

HCID 136360171HCID 136360171, compoundYield 89.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Stir, at room temperature under argon, a mixture of 2.0 g of 4-(6-chloro-1H-benzimidazol-2-yl)-9H-fluoren-9-one, 1.26 g of hydroxylamine hydrochloride and 2.48 g of sodium acetate in 100 ml of ethanol. The following day, evaporate the reaction medium to dryness under vacuum, take the residue up with 100 ml of dichloromethane and wash with 100 ml of water. The organic phase is dried over magnesium sulphate and evaporated to dryness under vacuum. After drying at 40° C. under vacuum, we obtain 1.88 g of 4-(6-chloro-1H-benzimidazol-2-yl)-9H-fluoren-9-one oxime (Z, E) in the form of a beige solid with the following characteristics:

Workup

  1. customThe following day, evaporate the reaction medium to dryness under vacuum
  2. washwash with 100 ml of water
  3. dry with materialThe organic phase is dried over magnesium sulphate
  4. customevaporated to dryness under vacuum
  5. customAfter drying at 40° C. under vacuum, we

Sources & evidence

ORD record
ord-1365a59ce6614e30b4d598dd2a25ae0e
Source dataset
uspto-grants-2010_03
Patent number
US07674795B2

Reaction notes

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