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

HRID 436107Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 436107
[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 994) 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-ede3604bcfdb40d5ba43e6e97b781f9c
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04007210

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