Sodium Acetate → HCID 86600713, compound

HRID 1820765Notes

Reaction equation

HRID 1820765 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-67d967d1ea434bbd8d982ea44ee59196
Source dataset
uspto-grants-2009_10
Patent number
US07605163B2

Reaction notes

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