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3-Ethoxycyclohex-2-ene-1-one → Spiro[2.5]octan-5-one

HRID 336620
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 336620
C(O[C:4]1[CH2:9][CH2:8][CH2:7][C:6](=[O:10])[CH:5]=1)C.[CH2:11]([Mg]Br)[CH3:12]>C(OCC)C.C(O[Ti](OC(C)C)(OC(C)C)OC(C)C)(C)C>[CH2:11]1[C:4]2([CH2:9][CH2:8][CH2:7][C:6](=[O:10])[CH2:5]2)[CH2:12]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 792163-Ethoxycyclohex-2-ene-1-oneHCID 178418443HCID 178418443, Verbindung

Produkt 1

HCID 12153480Spiro[2.5]octan-5-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178460666HCID 178460666, VerbindungKatalysatorHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

3-Ethoxycyclohex-2-enone (25 g) was dissolved in diethyl ether (500 mL), and tetraisopropoxytitanium (55 mL) was added, followed by the addition of ethyl magnesium bromide (3.0M in diethyl ether, 180 mL) over 30 minutes. The reaction was stirred at room temperature for another two hours, and quenched by the careful addition of water (250 mL). The mixture was filtered through diatomaceous earth, and rinsed with diethyl ether. The filtrate was transferred to a separatory funnel, the aqueous layer was drawn off, and p-toluenesulfonic acid monohydrate (2 g) was added to the organic layer, which was stirred at room temperature for two days. The reaction mixture was washed with saturated aqueous NaHCO3 and brine, then dried over Na2SO4. The mixture was filtered, and concentrated and chromatography on silica gel using 93/7 hexanes/ethyl acetate provided the title compound.

Aufarbeitung

  1. customquenched by the careful addition of water (250 mL)
  2. filtrationThe mixture was filtered through diatomaceous earth
  3. washrinsed with diethyl ether
  4. customThe filtrate was transferred to a separatory funnel
  5. additionp-toluenesulfonic acid monohydrate (2 g) was added to the organic layer, which
  6. stirringwas stirred at room temperature for two days
  7. washThe reaction mixture was washed with saturated aqueous NaHCO3 and brine
  8. dry with materialdried over Na2SO4
  9. filtrationThe mixture was filtered
  10. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-079cb49ef6104a1fb5c37f0ea4c986e5
Quelldatensatz
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08889675B2

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