Sodium Hydroxide → 7-(2,5-Dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acid

HRID 1646825

Reaktionsgleichung

Reaktionsgleichung von HRID 1646825
[OH-].[Na+].[CH3:3][O:4][C:5]1[C:10]([CH3:11])=[C:9]([CH3:12])[C:8]([O:13][CH3:14])=[C:7]([CH3:15])[C:6]=1[CH:16]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[CH2:17][CH2:18][CH2:19][CH2:20][C:21]([CH3:28])([CH3:27])[C:22]([O:24]CC)=[O:23]>C(O)C>[CH3:3][O:4][C:5]1[C:10]([CH3:11])=[C:9]([CH3:12])[C:8]([O:13][CH3:14])=[C:7]([CH3:15])[C:6]=1[CH:16]([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[CH2:17][CH2:18][CH2:19][CH2:20][C:21]([CH3:28])([CH3:27])[C:22]([OH:24])=[O:23]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 19088026Ethyl 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoate

Produkt 1

HCID 190880747-(2,5-Dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acidAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

3N Sodium hydroxide (9 ml) was added to a solution of 1.20 g (2.73 mmole) of ethyl 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoate in ethanol (12 ml), followed by stirring at 90° C. overnight (15 hours). After cooling by standing at room temperature, the ethanol was distilled off under reduced pressure, and the residue was made acid by adding a 10% aqueous phosphoric acid solution, followed by extraction of the product with isopropyl ether. The isopropyl ether layer was washed with aqueous sodium hydrochloride solution, dried (magnesium suflate) and evaporated to give 1.11 q (99%) of 7-(2,5-dimethoxy-3,4,6-trimethylphenyl)-2,2-dimethyl-7-phenylheptanoic acid. Its typical physical properties and nuclear magnetic resonance spectrum data are shown in Table 14.

Aufarbeitung

  1. temperatureAfter cooling
  2. customby standing at room temperature
  3. distillationthe ethanol was distilled off under reduced pressure
  4. additionby adding a 10% aqueous phosphoric acid solution
  5. extractionfollowed by extraction of the product with isopropyl ether
  6. washThe isopropyl ether layer was washed with aqueous sodium hydrochloride solution
  7. dry with materialdried (magnesium suflate)
  8. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-159e3818d89848a4bed8302dc9d8b313
Quelldatensatz
uspto-grants-1993_01
Patentnummer
US05180742

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