Acetonitrile → HCID 178496176, Verbindung

HRID 1642013Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1642013
CN1C(O[C:8](=[O:25])[C:9]2[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[C:11]([O:19][CH2:20][CH2:21][O:22][CH3:23])[C:10]=2[CH3:24])=CC=N1.C([N:28]([CH2:31][CH3:32])[CH2:29]C)C.CC(C)([OH:37])C#N.[C:39](#[N:41])C>>[CH3:23][O:22][CH2:21][CH2:20][O:19][C:11]1[C:10]([CH3:24])=[C:9]([CH:14]=[CH:13][C:12]=1[S:15]([CH3:18])(=[O:16])=[O:17])[C:8]([C:32]1[CH:39]=[N:41][N:28]([CH3:29])[C:31]=1[OH:37])=[O:25]

Komponenten

5

Edukt 4

HCID 6342AcetonitrileHCID 6406Acetone CyanohydrinHCID 8471TriethylamineHCID 667559103-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)benzoic acid 1-methyl-1H-pyrazol-5-yl ester

Produkt 1

HCID 178496176HCID 178496176, Verbindung

Versuchsvorschrift

3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)benzoic acid 1-methyl-1H-pyrazol-5-yl ester (7.8 g) was dissolved in acetonitrile (100 mL), and triethylamine (7.9 mL) and acetone cyanohydrin (0.87 mL) were added at room temperature. After stirring for 6 hours, the solvent was distilled off under reduced pressure. To the residue, ethyl acetate (100 mL) was added, followed by washing sequentially with 1N hydrochloric acid (50 mL), water and saturated brine, and drying over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was washed with hexane to obtain 4-(3-(2-methoxyethoxy)-2-methyl-4-(methylsulfonyl)benzoyl)-1-methyl-1H-pyrazol-5-ol (4.2 g).

Aufarbeitung

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionTo the residue, ethyl acetate (100 mL) was added
  3. washby washing sequentially with 1N hydrochloric acid (50 mL), water and saturated brine
  4. dry with materialdrying over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. washthe residue was washed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-362ea7becb62469ea53c78980f8d2cb3
Quelldatensatz
uspto-grants-2012_02
Patentnummer
US08119569B2

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