Hydroxyamine hydrochloride → HCID 117770185, compound

HRID 1526320Notes

Reaction equation

HRID 1526320 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]2[CH3:14])[C:4](=[O:15])[C:3]=1[CH:16]=O.Cl.[NH2:19][OH:20].C([O-])(=O)C.[Na+]>CO.O>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]2[CH3:14])[C:4](=[O:15])[C:3]=1[CH:16]=[N:19][OH:20]

Participants

5

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 117770386HCID 117770386, compound

Product 1

HCID 117770185HCID 117770185, compoundYield 92.1%

Reagents, catalysts & solvents 1

HCID 22242641Methanol--water (1/1)Solvent

Conditions

Temperature
75 °C

Procedure

A mixture of 4-chloro-1-(2-methylcyclohexyl)-2-oxo-1,2-dihydropyridine-3-carbaldehyde obtained in Step C (1.22 g), hydroxylamine hydrochloride (667 mg) and sodium acetate (787 mg) in methanol/water (4:1, 6.0 mL) was heated at 75° C. for 1 hr, and cooled to room temperature. The reaction mixture was poured into ice water, and the resulting solid was collected by filtration, washed with water, and dried under reduced pressure to give the title compound (1.19 g).

Workup

  1. temperaturecooled to room temperature
  2. filtrationthe resulting solid was collected by filtration
  3. washwashed with water
  4. customdried under reduced pressure

Sources & evidence

ORD record
ord-3269203b041b467ba4edfc6d987547e9
Source dataset
uspto-grants-2015_07
Patent number
US09085578B2

Reaction notes

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