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4-Fluorobenzyl bromide → 2-(5-(4-Fluoro-benzyl)-furan-2-yl)-[1,3]dioxolane

HRID 78244
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 78244
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[O:7][CH:8]=[CH:9][CH:10]=1.C([Li])CCC.[F:16][C:17]1[CH:24]=[CH:23][C:20]([CH2:21]Br)=[CH:19][CH:18]=1>O1CCCC1>[F:16][C:17]1[CH:24]=[CH:23][C:20]([CH2:21][C:8]2[O:7][C:6]([CH:2]3[O:3][CH2:4][CH2:5][O:1]3)=[CH:10][CH:9]=2)=[CH:19][CH:18]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 680214-Fluorobenzyl bromideHCID 2631582-Furyl-1,3-dioxolaneHCID 178418339Butyllithium

Produkt 1

HCID 592550712-(5-(4-Fluoro-benzyl)-furan-2-yl)-[1,3]dioxolaneAusbeute 51 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a tetrahydrofuran (50 mL) solution of 2-(1,3-dioxolan-2-yl-furan (5 g, 35.7 mmol) was added n-butyl lithium (15.6 mL, 2.64 M hexane solution, 41.1 mmol) at −78° C., which was stirred for 1 hour at that temperature. A tetrahydrofuran solution of 4-fluorobenzyl bromide (6.9 g, 36.5 mmol) was added dropwise to this mixture, which was stirred for another hour at −78° C. The mixture was raised to room temperature and partitioned into ethyl acetate and a saturated ammonium chloride aqueous solution. The organic layer was separated, washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:10 to 1:3) to obtain the title compound (4.51 g, 51%).

Aufarbeitung

  1. stirringwas stirred for another hour at −78° C
  2. custompartitioned into ethyl acetate
  3. customThe organic layer was separated
  4. washwashed with saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under a reduced pressure
  8. customthe residue was purified by silica gel column chromatography (ethyl acetate:heptane=1:10 to 1:3)

Quellen und Nachweise

ORD-Eintrag
ord-ec9e12fe4aab477799439ea67d534541
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08841327B2

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