Reaktion #814371

ord-f647501c2b81467fa27a638a218d4aad

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture is then concentrated under reduced pressure to a residue
  2. 2
    workup.STIRRINGThe residue is stirred in about 150 mL of water
  3. 3
    Extraktionthe mixture is extracted with three 150 mL portions of diethyl ether
  4. 4
    TrocknenThe combined extracts are dried with magnesium sulfate
  5. 5
    Filtrationfiltered
  6. 6
    EinengenThe filtrate is concentrated under reduced pressure

Vorschrift

A mixture of 16.7 grams (0.07 mole) of 8-trimethylsilylethynyl-1,4-dioxaspiro[4.5]decane and 1.1 grams (0.07 mole) of potassium carbonate in 200 mL of methanol is stirred at ambient temperature for about one hour. The reaction mixture is then concentrated under reduced pressure to a residue. The residue is stirred in about 150 mL of water, and the mixture is extracted with three 150 mL portions of diethyl ether. The combined extracts are dried with magnesium sulfate and filtered. The filtrate is concentrated under reduced pressure, yielding 8-ethynyl-1,4-dioxaspiro[4.5]decane.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05712281uspto-grants-1998_01