Methanol → HCID 21485772, Verbindung

HRID 1077141

Reaktionsgleichung

Reaktionsgleichung von HRID 1077141
[C:1]([O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][CH2:13][C:14](=[O:22])[CH2:15][CH2:16]N(CC)CC)[CH:8]=[CH:9][CH:10]=1)(=[O:3])[CH3:2].C(OC1C=C(CCCC(=O)C=C)C=CC=1)(=O)C.[CH3:40][CH:41]1[C:45](=[O:46])[CH2:44][CH2:43][C:42]1=[O:47].CO>[OH-].[K+].C(Cl)(Cl)Cl>[C:1]([O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][CH2:13][C:14](=[O:22])[CH2:15][CH2:16][C:41]2([CH3:40])[C:45](=[O:46])[CH2:44][CH2:43][C:42]2=[O:47])[CH:8]=[CH:9][CH:10]=1)(=[O:3])[CH3:2]

Komponenten

7

Edukt 4

HCID 887MethanolHCID 130052-Methyl-1,3-cyclopentanedioneHCID 214854206-m-Acetoxyphenyl-1-diethylaminohexan-3-oneHCID 214855806-m-Acetoxyphenylhex-1-en-3-one

Produkt 1

HCID 21485772HCID 21485772, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 14797Potassium HydroxideLösungsmittel

Versuchsvorschrift

Reflux a mixture of 6-(m-acetoxyphenyl)-1-diethylaminohexan-3-one and 6-(m-acetoxyphenyl)hex-1-en-3-one (1 g), with 2-methylcyclopentane-1,3-dione (1.5 g) in 0.12% methanolic potassium hydroxide (6 cc) for 18 hours. Remove methanol (2 cc) under reduced pressure and add chloroform (60 cc). Wash the solution in turn with dilute sulfuric acid (25 cc), saturated potassium bicarbonate solution, and brine; dry and evaporate the solvent. The product (0.8 g) is the adduct 2-(6-m-acetoxyphenyl-3-oxohexyl)-2-methylcyclopentane-1,3-dione in admixture with some of the corresponding free phenol; infrared absorption: 2.86 to 3.08 (broad low-intensity band), 5.71, 5.81, 5.85, and 8.26 μ.

Aufarbeitung

  1. temperatureReflux
  2. washWash the solution in turn with dilute sulfuric acid (25 cc), saturated potassium bicarbonate solution, and brine
  3. customdry
  4. customevaporate the solvent
  5. customabsorption

Quellen und Nachweise

ORD-Eintrag
ord-8782780bea62495b8605cb452e75635c
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03959322

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