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Allyl bromide → 4-(Allyloxy)-2,3-dihydro-1H-indene

HRID 13911
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 13911
C(=O)([O-])[O-].[K+].[K+].[CH2:7]1[C:15]2[CH:14]=[CH:13][CH:12]=[C:11]([OH:16])[C:10]=2[CH2:9][CH2:8]1.[CH2:17](Br)[CH:18]=[CH2:19]>CN(C)C=O.O>[CH2:19]([O:16][C:11]1[CH:12]=[CH:13][CH:14]=[C:15]2[C:10]=1[CH2:9][CH2:8][CH2:7]2)[CH:18]=[CH2:17]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 742334-Hydroxyindan

Produkt 1

HCID 685848044-(Allyloxy)-2,3-dihydro-1H-indene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a suspension of potassium carbonate (23.49 g, 0.170 mol) in N,N-dimethylformamide (350 mL) was added indan-4-ol (7.60 g, 0.057 mol) followed by allyl bromide (8.22 g, 0.068 mol) and the reaction mixture was allowed to stir at room temperature for 12 h. The reaction mixture was diluted with water (1000 mL) to dissolve any solids and extracted with diethyl ether (3×250 mL). The combined organic layers were washed with water (4×500 mL), aqueous sodium chloride (400 mL), dried (magnesium sulfate) and the solvent was removed in vacuo to give 4-(allyloxy)indane. The allyl ether was dissolved in mesitylene (40 mL) and heated at reflux for 8 h. Removal of the solvent in vacuo provided 5-allylindan-4-ol, which was re-dissolved in N,N-dimethylformamide (250 mL). Potassium carbonate (14.28 g, 0.103 mol), benzyl bromide (6.48 g, 0.038 mol), and tetrabutylammonium iodide (2.54 g, 0.007 mol) were added to the reaction mixture. The reaction mixture was allowed to stir at room temperature for 12 h. The reaction mixture was diluted with water (1000 mL) to dissolve any solids and extracted with diethyl ether (3×250 mL). The combined organic layers were washed with water (4×500 mL), aqueous sodium chloride (400 mL), dried (magnesium sulfate) and the solvent was removed in vacuo to give a crude oil. Purification by flash column chromatography (silica, ethyl acetate:hexanes 1:9) provided 10.22 g (68%) of 5-allyl-2,3-dihydro-1H-inden-4-yl benzyl ether as a pale yellow oil. Rf=0.45 (silica, ethyl acetate:hexanes 1:19); Anal. calcd. for C19H20O: C, 86.32; H, 7.63. Found: C, 85.90; H, 7.49.

Aufarbeitung

  1. dissolutionto dissolve any solids
  2. extractionextracted with diethyl ether (3×250 mL)
  3. washThe combined organic layers were washed with water (4×500 mL), aqueous sodium chloride (400 mL)
  4. dry with materialdried (magnesium sulfate)
  5. customthe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-0073296be60345cca74feff931ba75ef
Quelldatensatz
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07728155B2

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