Hydroxyamine hydrochloride → HCID 73863356, compound

HRID 649756Notes

Reaction equation

HRID 649756 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-35cdc1ba046b4f50a17d1918303c7862
Source dataset
uspto-grants-2001_08
Patent number
US06271223B1

Reaction notes

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