Sodium Hydroxide → HCID 22759245, Verbindung

HRID 460858Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 460858
[C:1]([CH:4]([CH2:16][CH2:17][CH2:18][CH:19]([OH:32])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[CH:23]=1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([O:13]CC)=[O:12])(=[O:3])[CH3:2].[OH-].[Na+]>O.CO>[C:1]([CH:4]([CH2:16][CH2:17][CH2:18][CH:19]([OH:32])[CH2:20][O:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:30])([F:31])[F:29])[CH:23]=1)[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12])(=[O:3])[CH3:2]

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 22759220HCID 22759220, Verbindung

Produkt 1

HCID 22759245HCID 22759245, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of ethyl 8-acetyl-12-hydroxy-13-(3-trifluoromethylphenoxy)tridecanoate (17.4 g., 0.038 mole) and sodium hydroxide (4 g., 0.1 mole) in water (30 ml.) and methanol (120 ml.) is heated at 60° for 16 hours. Most of the methanol is then removed by distillation in vacuo. The residue is dissolved in 150 ml. of water and extracted with ether. The aqueous solution is acidified with concentrated hydrochloric acid. The oily product is taken up in ether and dried over sodium sulfate. Ether is evaporated in vacuo to leave the title compound as a viscous oil weighing 12.9 g. The product is purified by column chromatography on 200 g. of silica gel with 2% methanol in chloroform as eluant; pmr (CDCl3) δ 2.10 (3H, s CH3CO); 3.95 (3H, broad s CHO and CH2O); 6.75 (2H, s OH and CO2H).

Aufarbeitung

  1. customMost of the methanol is then removed by distillation in vacuo
  2. dissolutionThe residue is dissolved in 150 ml
  3. extractionof water and extracted with ether
  4. dry with materialdried over sodium sulfate
  5. customEther is evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3666abe8ade24cee92326c4a2a5b852b
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04061643

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