Hydroxylamine HCl → HCID 66864640, compound

HRID 1929281Notes

Reaction equation

HRID 1929281 reaction equation
[Cl-].O[NH3+].[CH:4]1([C:7](=[O:28])[C:8](=[CH:24][N:25](C)C)[C:9]([C:11]2[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[C:13]([NH:21][CH3:22])[C:12]=2[CH3:23])=[O:10])[CH2:6][CH2:5]1>C(O)C>[CH:4]1([C:7]2[O:28][N:25]=[CH:24][C:8]=2[C:9](=[O:10])[C:11]2[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[C:13]([NH:21][CH3:22])[C:12]=2[CH3:23])[CH2:6][CH2:5]1

Participants

4

Reactant 2

HCID 21645Hydroxylamine HClHCID 66863658HCID 66863658, compound

Product 1

HCID 66864640HCID 66864640, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

0.19 g (2.8 mmol) of hydroxylammonium chloride was added to a solution of 0.85 g (2.3 mmol) of 1-cyclopropyl-2-(dimethylaminomethylidene)-3-(3-methylamino-2-methyl-4-methylsulfonylphenyl)propane-1,3-dione in 100 ml of ethanol. The mixture was stirred for 3 h at RT, and the solvent was removed in vacuo. The residue was taken up in CH2Cl2, washed with 10% strength H2SO4 and dried over MgSO4. The solvent was removed in vacuo, and the residue was purified by column chromatography on silica gel. This gave 0.50 g of product in 95% purity.

Workup

  1. customthe solvent was removed in vacuo
  2. washwashed with 10% strength H2SO4
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed in vacuo
  5. customthe residue was purified by column chromatography on silica gel

Sources & evidence

ORD record
ord-8e0f2e47295b41a6942005bb4e3597f8
Source dataset
uspto-grants-2012_05
Patent number
US08188009B2

Reaction notes

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