Sodium Acetate → HCID 86600713, compound

HRID 2251221Notes

Reaction equation

HRID 2251221 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([C:30](=O)[CH3:31])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:29])[C:15]2[CH:20]=[C:19]([S:21]([CH3:24])(=[O:23])=[O:22])[CH:18]=[CH:17][C:16]=2[O:25][CH:26]([CH3:28])[CH3:27])[CH2:10][CH2:9]1.Cl.[CH3:34][O:35][NH2:36].C([O-])(=O)C.[Na+]>C(O)C.O>[CH3:34][O:35][N:36]=[C:30]([C:4]1[CH:5]=[CH:6][C:7]([N:8]2[CH2:9][CH2:10][N:11]([C:14](=[O:29])[C:15]3[CH:20]=[C:19]([S:21]([CH3:24])(=[O:22])=[O:23])[CH:18]=[CH:17][C:16]=3[O:25][CH:26]([CH3:28])[CH3:27])[CH2:12][CH2:13]2)=[C:2]([F:1])[CH:3]=1)[CH3:31]

Participants

6

Reactant 3

HCID 517045Sodium AcetateHCID 521874O-Methylhydroxylamine hydrochlorideHCID 11488045HCID 11488045, compound

Product 1

HCID 86600713HCID 86600713, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent2×

Procedure

0.12 mmol of 1-{3-Fluoro-4-[4-(2-isopropoxy-5-methanesulfonyl-benzoyl)-piperazin-1-yl]-phenyl}-ethanone was dissolved in 1 ml of a 1:1 mixture of ethanol and water. 0.8 mmol of O-methyl-hydroxylamine hydrochloride was added, followed by 8.4 mmol of sodium acetate. The slurry was stirred overnight at room temperature, diluted with water, extracted with ethyl acetate, dried and concentrated. The resulting gum was triturated with diethyl ether/heptane to yield the title compound as a colorless solid. MS (m/e): 492.3 (MH+, 100%)

Workup

  1. extractionextracted with ethyl acetate
  2. customdried
  3. concentrationconcentrated
  4. customThe resulting gum was triturated with diethyl ether/heptane

Sources & evidence

ORD record
ord-bf7adee65c5f4f7e8e218e609568cf5d
Source dataset
uspto-grants-2008_01
Patent number
US07319099B2

Reaction notes

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