Reaktion #1850115

ord-8f47fd815f2a4ae19a3b534dd8a00920

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is heated
  2. 2
    Einengenconcentrated under vacuum
  3. 3
    Temperaturheated for one hour
  4. 4
    Temperaturunder reflux
  5. 5
    Sonstigethe mixture is evaporated to dryness under vacuum
  6. 6
    Sonstigethe clear solution is decanted from the dark residue
  7. 7
    Temperaturcooling of the solution

Vorschrift

A suspension of 6.0 g of 7-methoxyindole-2carboxylic acid in 100 ml of toluene is combined with 4.3 ml of thionyl chloride; the mixture is heated under stirring for 3 hours to 90° C., then concentrated under vacuum. The residue is combined with 50 ml of n-butanol and heated for one hour under reflux Then the mixture is evaporated to dryness under vacuum, the oily residue is boiled with 60 ml of petroleum ether, the clear solution is decanted from the dark residue, and cooling of the solution yields 4.1 g of 7-methoxyindole-2-carboxylic acid n-butyl ester, mp 66°-69° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04835175uspto-grants-1989_05