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Hydrochloric Acid → HCID 66602549, Verbindung

HRID 2097472
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2097472
CO.[Br:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH:11]([F:13])[F:12])=[C:6]([O:14]CC2CC2)[CH:5]=1.Cl>O>[Br:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH:11]([F:12])[F:13])=[C:6]([OH:14])[CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 100172571-Bromo-3-cyclopropylmethoxy-4-difluoromethoxybenzene

Produkt 1

HCID 66602549HCID 66602549, VerbindungAusbeute 101,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 60 ml of methanol solution containing 5.80 g (19.7 mmol) of 4-bromo-2-cyclopropylmethoxy-1-difluoromethoxybenzene (see WO 2004033430) was added 60 ml of conc. hydrochloric acid, and the mixture was refluxed for 5 hours. After completion of the reaction, 60 ml of water was added to the reaction mixture, and the mixture was extracted with diethyl ether. The organic layer after separation was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=4:1 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 4.80 g of the title compound as a slightly yellowish oil substantially quantitatively.

Aufarbeitung

  1. temperaturethe mixture was refluxed for 5 hours
  2. additionwas added to the reaction mixture
  3. extractionthe mixture was extracted with diethyl ether
  4. customThe organic layer after separation
  5. washwas washed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. additionthe fractions containing the desired compound
  9. concentrationwere concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-60e6af96f44645dbb01690a0ce83e122
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08450319B2

Notizen zur Reaktion

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