Triethylamine → HCID 21449437, Verbindung

HRID 596961

Reaktionsgleichung

Reaktionsgleichung von HRID 596961
[CH3:1][C:2]1([CH3:10])[C:4]([CH3:6])([CH3:5])[CH:3]1[C:7](Cl)=[O:8].[C:11]([CH:13]([OH:27])[C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([O:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:15]=1)#[CH:12].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:10])[C:4]([CH3:6])([CH3:5])[CH:3]1[C:7]([O:27][CH:13]([C:11]#[CH:12])[C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([O:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:15]=1)=[O:8]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 110410022,2,3,3-Tetramethylcyclopropane-1-carbonyl chlorideHCID 129190923-Phenoxy-alpha-ethynylbenzylalcohol

Produkt 1

HCID 21449437HCID 21449437, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

2,2,3,3-Tetramethylcyclopropanoyl chloride (3.05 g) was added with stirring to a solution of α-ethynyl-3-phenoxybenzylalcohol (4.8 g) and triethylamine (2.16 g) in dry toluene (70 ml) at 10° C. The solution was allowed to attain room temperature and stirred for 16 hours. The mixture was filtered and the solvent removed from the filtrate under reduced pressure. The residue was washed with 5% sulphuric acid, followed by saturated sodium bicarbonate solution and finally purified by chromatography on silica gel using toluene as eluent to give the desired product as an oil nD20 1.5455.

Aufarbeitung

  1. customto attain room temperature
  2. filtrationThe mixture was filtered
  3. customthe solvent removed from the filtrate under reduced pressure
  4. washThe residue was washed with 5% sulphuric acid
  5. customfinally purified by chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-62a9ecd109444ba88607cfac655e7ce0
Quelldatensatz
uspto-grants-1977_03
Patentnummer
US04012522

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