Potassium Hydroxide → 2-Ethyl-2-methyl-6-[(4,6-diphenyl-2-pyridyl)oxy]hexanoic acid

HRID 2380354

Reaktionsgleichung

Reaktionsgleichung von HRID 2380354
[CH2:1]([C:3]([CH3:32])([CH2:9][CH2:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:17]=[C:16]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:15]=1)[C:4]([O:6]CC)=[O:5])[CH3:2].[OH-].[K+]>O.C(O)C>[CH2:1]([C:3]([CH3:32])([CH2:9][CH2:10][CH2:11][CH2:12][O:13][C:14]1[CH:19]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:17]=[C:16]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:15]=1)[C:4]([OH:6])=[O:5])[CH3:2]

Komponenten

5

Edukt 2

HCID 14797Potassium HydroxideHCID 18987342Ethyl 2-ethyl-2-methyl-6-[(4,6-diphenyl-2-pyridyl)oxy]hexanoate

Produkt 1

HCID 189872252-Ethyl-2-methyl-6-[(4,6-diphenyl-2-pyridyl)oxy]hexanoic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

The procedure in Example 6 is followed but using ethyl 2-ethyl-2-methyl-6-[(4,6-diphenyl-2-pyridyl)oxy]hexanoate (3.6 g), potassium hydroxide pellets (0.95 g) dissolved in distilled water (20 cc) and ethanol (50 cc). The reaction mixture is refluxed for 120 hours. The product is purified by chromatography under pressure on silica gel (30-60 mm; eluent: n-hexane-ethyl acetate 75-25) and then by recrystallisation in an n-hexane-ethyl acetate (2-1) mixture (40 cc), white crystals (m.p.=119°-120° C.)

Aufarbeitung

  1. temperatureThe reaction mixture is refluxed for 120 hours
  2. customThe product is purified by chromatography under pressure on silica gel (30-60 mm; eluent: n-hexane-ethyl acetate 75-25)
  3. customby recrystallisation in an n-hexane-ethyl acetate (2-1) mixture (40 cc), white crystals (m.p.=119°-120° C.)

Quellen und Nachweise

ORD-Eintrag
ord-fbaf54f3fff84a4fae28926f8847d678
Quelldatensatz
uspto-grants-1994_11
Patentnummer
US05366982

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