3,4-dihydro-2H-pyran → 2-[(4,4-Dimethyloct-1-YN-3-YL)oxy]oxane

HRID 225358Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 225358
[CH3:1][C:2]([CH3:11])([CH2:7][CH2:8][CH2:9][CH3:10])[CH:3]([OH:6])[C:4]#[CH:5].[O:12]1[CH:17]=[CH:16][CH2:15][CH2:14][CH2:13]1>P(Cl)(Cl)(Cl)=O.C(N(CC)CC)C>[CH3:1][C:2]([CH3:11])([CH2:7][CH2:8][CH2:9][CH3:10])[CH:3]([O:6][CH:13]1[CH2:14][CH2:15][CH2:16][CH2:17][O:12]1)[C:4]#[CH:5]

Komponenten

5

Edukt 2

HCID 80803,4-dihydro-2H-pyranHCID 145163694,4-Dimethyl-1-octyn-3-ol

Produkt 1

HCID 145163702-[(4,4-Dimethyloct-1-YN-3-YL)oxy]oxane

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8471TriethylamineKatalysatorHCID 24813Phosphorus oxychlorideKatalysator

Versuchsvorschrift

To a solution of 23.1 g. (0.150 mole) of 4,4-dimethyl-1-octyn-3-ol (Example 149) in 126 g. of freshly distilled dihydropyran is added 1 drop of phosphorus oxychloride and the solution is maintained at ambient temperature in a tightly stoppered flask for 20 hours. Five drops of triethylamine are then added and the mixture is evaporated in vacuo to an oil. The oil is chromatographed on 600 g. of silica gel and the product is eluted with 5% ethyl acetate in benzene yielding a colorless oil.

Aufarbeitung

  1. customthe mixture is evaporated in vacuo to an oil
  2. customThe oil is chromatographed on 600 g
  3. washof silica gel and the product is eluted with 5% ethyl acetate in benzene yielding a colorless oil

Quellen und Nachweise

ORD-Eintrag
ord-8780e8d28d93486494bc8f93693a19c5
Quelldatensatz
uspto-grants-1980_11
Patentnummer
US04236027

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