Hydroxyamine hydrochloride → HCID 73863356, compound

HRID 1168598Notes

Reaction equation

HRID 1168598 reaction equation
[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][C:9](=O)[C:8]2[N:12]([CH3:15])[CH:13]=[CH:14][C:7]=2[S:6]1(=[O:17])=[O:16].Cl.[NH2:19][OH:20].C([O-])(=O)C.[K+]>CO>[Cl:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][C:9](=[N:19][OH:20])[C:8]2[N:12]([CH3:15])[CH:13]=[CH:14][C:7]=2[S:6]1(=[O:17])=[O:16]

Participants

5

Reactant 3

HCID 443297Hydroxyamine hydrochloride2×HCID 517044Potassium Acetate2×HCID 22065897HCID 22065897, compound

Product 1

HCID 73863356HCID 73863356, compoundYield 88%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A suspension of 300 mg (1.08 mmol) of Compound 16, 113 mg (1.62 mmol) of hydroxylamine hydrochloride and 159 mg (1.62 mmol) of potassium acetate in 10 ml of methanol was refluxed for 7 hours. To the reaction mixture, 75 mg (1.08 mmol) of hydroxylamine hydrochloride and 106 mg (1.08 mmol) of potassium acetate were added, followed by further refluxing for 13 hours. Post treatment and purification were conducted as in Example 9, whereby 277 mg of the title compound were obtained (yield: 88%).

Workup

  1. temperaturewas refluxed for 7 hours
  2. temperatureby further refluxing for 13 hours
  3. customPost treatment and purification

Sources & evidence

ORD record
ord-1d3837822ef146d99c90e2cd0531fa08
Source dataset
uspto-grants-2003_09
Patent number
US06624314B2

Reaction notes

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