Hydroxylamine HCl → HCID 86628504, compound

HRID 546665Notes

Reaction equation

HRID 546665 reaction equation
C([O-])(=O)C.[Na+].[Cl-].[OH:7][NH3+:8].[F:9][C:10]1[CH:11]=[C:12]([C:16]2([CH:41]=O)[CH2:21][CH2:20][CH2:19][N:18]3[N:22]=[C:23](/[CH:25]=[CH:26]/[C:27]4[CH:32]=[CH:31][C:30]([N:33]5[CH:37]=[C:36]([CH3:38])[N:35]=[CH:34]5)=[C:29]([O:39][CH3:40])[CH:28]=4)[N:24]=[C:17]23)[CH:13]=[CH:14][CH:15]=1.O.C(=O)(O)[O-].[Na+]>C(O)C.C(OCC)(=O)C>[F:9][C:10]1[CH:11]=[C:12]([C:16]2([CH:41]=[N:8][OH:7])[CH2:21][CH2:20][CH2:19][N:18]3[N:22]=[C:23](/[CH:25]=[CH:26]/[C:27]4[CH:32]=[CH:31][C:30]([N:33]5[CH:37]=[C:36]([CH3:38])[N:35]=[CH:34]5)=[C:29]([O:39][CH3:40])[CH:28]=4)[N:24]=[C:17]23)[CH:13]=[CH:14][CH:15]=1

Participants

7

Reactant 4

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 86585896Sodium bicarbonate waterHCID 86628503HCID 86628503, compound

Product 1

HCID 86628504HCID 86628504, compoundYield 99.8%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

Sodium acetate (58.7 mg) and hydroxylammonium chloride (49.8 mg) were added to a solution of 8-(3-fluorophenyl)-2-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-5,6,7,8-tetrahydro[1,2,4]triazolo[1,5-a]pyridine-8-carbaldehyde (164 mg) in ethanol (10 mL), and the reaction solution was stirred at room temperature for five hours. Ethyl acetate and saturated sodium bicarbonate water were added to the reaction solution and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain 169 mg of the title compound. The property value of the compound is as follows.

Workup

  1. customthe organic layer was separated
  2. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-a5d7231bc73549a08d272da209412952
Source dataset
uspto-grants-2011_05
Patent number
US07935815B2

Reaction notes

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