Acetone → HCID 66628195, Verbindung

HRID 386533

Reaktionsgleichung

Reaktionsgleichung von HRID 386533
[OH-:1].[Na+].[Br:3][C:4]1[C:5]([CH3:10])=[N:6][NH:7][C:8]=1[CH3:9].Cl[C:12](Cl)(Cl)[C:13](O)([CH3:15])[CH3:14].CC(C)=[O:21]>>[Br:3][C:4]1[C:5]([CH3:10])=[N:6][N:7]([C:13]([CH3:15])([CH3:14])[C:12]([OH:21])=[O:1])[C:8]=1[CH3:9]

Komponenten

5

Edukt 4

HCID 180AcetoneHCID 5977ChlorobutanolHCID 14798Sodium HydroxideHCID 769374-bromo-3,5-dimethyl-1H-pyrazole

Produkt 1

HCID 66628195HCID 66628195, Verbindung

Versuchsvorschrift

To a cold (0° C.), well stirred suspension of NaOH (1.6 g, 40 mmoles) and 4-bromo-3,5-dimethylpyrazole (1.75 g, 10 mmoles) in acetone (100 mL), was added 2-(trichloromethyl)-propan-2-ol (3.54 g, 20 mmoles) portion-wise over 1 hour. The mixture was allowed to warm to room temperature overnight. The solvent was evaporated under reduced pressure. The residue was dissolved in water (100 mL) and washed with ether (50 mL). The aqueous phase was separated and acidified with conc. HCl to pH=3. The mixture was extracted with CH2Cl2 (3×50 mL) and the combined organics dried over Na2SO4. A colorless oil was obtained after the removal of the solvent under reduced pressure. MS(DCI+) m/z 263 (M+H)+.

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in water (100 mL)
  3. washwashed with ether (50 mL)
  4. customThe aqueous phase was separated
  5. extractionThe mixture was extracted with CH2Cl2 (3×50 mL)
  6. dry with materialthe combined organics dried over Na2SO4
  7. customA colorless oil was obtained
  8. customafter the removal of the solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-4947e44d8de84158927b1560771772bc
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08372841B2

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