Potassium Carbonate → HCID 10820667, Verbindung

HRID 918375Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 918375
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][C:9]#[N:10].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(=O)([O-])[O-].[K+].[K+]>CCOCC.O1CCCC1>[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][NH2:10]

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 544562(Tetrahydro-pyran-2-yloxy)-acetonitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 10820667HCID 10820667, VerbindungAusbeute 93,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 35 g of tetrahydropyran-2-yloxy acetonitrile in 100 ml of ether is added dropwise to a slurry of 10 g of lithium aluminum hydride in 300 ml of ether and 100 ml of tetrahydrofuran. The slurry is refluxed for 210 minutes, cooled, and 25 ml of sat. potassium carbonate solution is added at a rate that maintains gentle reflux. After 90 minutes the slurry is filtered and the solid is washed with ether. The filtrate is evaporated in vacuo and distilled to give 33.6 g of 2-(tetrahydropyran-2-yloxy)ethylamine, boiling point 41.5°-46°C at 0.5-0.8 mm.

Aufarbeitung

  1. temperatureThe slurry is refluxed for 210 minutes
  2. temperaturecooled
  3. filtrationAfter 90 minutes the slurry is filtered
  4. washthe solid is washed with ether
  5. customThe filtrate is evaporated in vacuo
  6. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-3d5c6c31f5104a13a8ad6518a76949fc
Quelldatensatz
uspto-grants-1976_07
Patentnummer
US03971772

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