Hydrochloric Acid → 2,3,5,6-Tetrafluoro-4-[(1-methylethoxy)methyl]-benzyl alcohol

HRID 1088322

Reaktionsgleichung

Reaktionsgleichung von HRID 1088322
[Na].[CH:2]([OH:5])([CH3:4])[CH3:3].Br[CH2:7][C:8]1[C:15]([F:16])=[C:14]([F:17])[C:11]([CH2:12][OH:13])=[C:10]([F:18])[C:9]=1[F:19].Cl>O>[F:17][C:14]1[C:15]([F:16])=[C:8]([CH2:7][O:5][CH:2]([CH3:4])[CH3:3])[C:9]([F:19])=[C:10]([F:18])[C:11]=1[CH2:12][OH:13]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 5360545SodiumHCID 11265752(4-(Bromomethyl)-2,3,5,6-tetrafluorophenyl)methanol

Produkt 1

HCID 147188942,3,5,6-Tetrafluoro-4-[(1-methylethoxy)methyl]-benzyl alcohol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

Sodium (1.0 g) was added to dry isopropanol (200 cm3), maintained at 40° C. under an atmosphere of dry nitrogen. After dissolution was complete, 4-(bromomethyl)-2,3,5,6-tetrafluorobenzyl alcohol (10.9 g) was added and the reaction was stirred for 16 hours, at the ambient temperature. The reaction mixture was poured into water, acidified with dilute aqueous hydrochloric acid, and extracted into ethyl acetate. The combined organic extracts were washed with water, dried over anhydrous magnesium sulphate, and concentrated by evaporation of the solvent under reduced pressure. The residue was combined with the product of a similar reaction and distilled under reduced pressure to give 2,3,5,6-tetrafluoro-4-[(1-methylethoxy)methyl]-benzyl alcohol (0.8 g).

Aufarbeitung

  1. dissolutionAfter dissolution
  2. extractionextracted into ethyl acetate
  3. washThe combined organic extracts were washed with water
  4. dry with materialdried over anhydrous magnesium sulphate
  5. concentrationconcentrated by evaporation of the solvent under reduced pressure
  6. customThe residue was combined with the product of a similar reaction
  7. distillationdistilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-53065047eea7425eb5219f15b7b34fe2
Quelldatensatz
uspto-grants-1990_10
Patentnummer
US04962109

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