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Ethyl phenylacetate → Ethyl 3-(2,3-dihydrobenzofuran-5-yl)-2-phenylpropionate

HRID 1636608
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1636608
C[Si](C)(C)[N-][Si](C)(C)C.[Li+].C[Si](C)(C)N[Si](C)(C)C.C([Li])CCC.[C:25]1([CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.Br[CH2:38][C:39]1[CH:40]=[CH:41][C:42]2[O:46][CH2:45][CH2:44][C:43]=2[CH:47]=1>O1CCCC1.O>[O:46]1[C:42]2[CH:41]=[CH:40][C:39]([CH2:38][CH:31]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:32]([O:34][CH2:35][CH3:36])=[O:33])=[CH:47][C:43]=2[CH2:44][CH2:45]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 7590Ethyl phenylacetateHCID 13838HexamethyldisilazaneHCID 2733832Lithium hexamethyldisilazaneHCID 220048075-(Bromomethyl)-2,3-dihydrobenzofuranHCID 178418339Butyllithium

Produkt 1

HCID 22004839Ethyl 3-(2,3-dihydrobenzofuran-5-yl)-2-phenylpropionate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

To a solution of lithium hexamethyldisilazide solution, prepared from 1,1,1,3,3,3-hexamethyldisilazane (37.4 g, 0.232 mol), n-butyllithium (127 mL, 1.6 M hexane solution) and tetrahydrofuran (150 mL), was added a solution of ethyl phenylacetate (33.3 g, 0.203 mol) in tetrahydrofuran (20 mL) at -78° C. The mixture was stirred for 15 minutes and then a solution of 5-bromomethyl-2,3-dihydrobenzofuran (41.0 g, 0.193 mol) in tetrahydrofuran (50 mL) was added. The mixture was stirred for further 20 minutes, diluted with water and warmed up to room temperature. The product was extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to afford the title compound as an oily product (yield 54.5 g, 95%).

Aufarbeitung

  1. stirringThe mixture was stirred for further 20 minutes
  2. extractionThe product was extracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated
  6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)

Quellen und Nachweise

ORD-Eintrag
ord-e97a7ba2af0b4130921f553cfb28c8f9
Quelldatensatz
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06034239

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