Lithium hydroxide, monohydrate → 2-(3,4,5-Trimethoxyphenylethynyl)pyridine-4-carboxylic Acid

HRID 1634899Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1634899
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13]#[C:14][C:15]2[CH:20]=[C:19]([C:21]([O:23]CC)=[O:22])[CH:18]=[CH:17][N:16]=2)[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].O.[OH-].[Li+]>CO>[CH3:12][O:11][C:7]1[CH:6]=[C:5]([C:13]#[C:14][C:15]2[CH:20]=[C:19]([C:21]([OH:23])=[O:22])[CH:18]=[CH:17][N:16]=2)[CH:4]=[C:3]([O:2][CH3:1])[C:8]=1[O:9][CH3:10]

Komponenten

4

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 18674974Ethyl 2-(3,4,5-trimethoxyphenylethynyl)pyridine-4-carboxylate

Produkt 1

HCID 186750082-(3,4,5-Trimethoxyphenylethynyl)pyridine-4-carboxylic Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Ethyl 2-(3,4,5-trimethoxyphenylethynyl)pyridine-4-carboxylate (1.40 g) was suspended in methanol (100 mL), to the suspension lithium hydroxide hydrate (189 mg) was added, and the mixture was stirred at room temperature for 4 hours. The reaction mixture was concentrated under reduced pressure, water was added to the residue and the resultant mixture was neutralized with 1 M hydrochloric acid. After the reaction mixture was cooled with ice, crystals precipitated were collected by filtration to obtain the title compound as colorless crystals.

Aufarbeitung

  1. additionwas added
  2. concentrationThe reaction mixture was concentrated under reduced pressure, water
  3. additionwas added to the residue
  4. temperatureAfter the reaction mixture was cooled with ice, crystals
  5. customprecipitated
  6. filtrationwere collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-91c4c7b83f194cd29e276cd14a143adc
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06509329B1

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