Hydrochloric Acid → (E)-2-(3-Chloroprop-1-en-1-yl)-1,4-difluorobenzene
Reaktionsgleichung
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1/[CH:9]=[CH:10]/[CH2:11]O.[ClH:13]>O1CCOCC1>[Cl:13][CH2:11]/[CH:10]=[CH:9]/[C:3]1[CH:4]=[C:5]([F:8])[CH:6]=[CH:7][C:2]=1[F:1]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
A mixture of (2E)-3-(2,5-difluorophenyl)prop-2-en-1-ol (Intermediate 70, 700 mg, 4.12 mmol), 1,4-dioxane (5 mL), and hydrochloric acid (12.1 M, 1 mL) was heated in the microwave at 100° C. for 3 hours. It was concentrated to dryness under reduced pressure, the residue taken up in ethyl acetate (10 mL), washed with water (1×10 mL), saturated sodium bicarbonate solution, brine and dried over sodium sulfate. The solvent was removed under reduced pressure to give 688 mg (89% yield) of product as a yellow oil.
Aufarbeitung
- concentrationIt was concentrated to dryness under reduced pressure
- washwashed with water (1×10 mL), saturated sodium bicarbonate solution, brine
- dry with materialdried over sodium sulfate
- customThe solvent was removed under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-9eb8c6f0374149daa4e9d08b85e6baff
- Quelldatensatz
- uspto-grants-2012_02
- Patentnummer
- US08124602B2
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