Reaktion #215390

ord-b1c815612f6b4507bd14234b027a76db

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturIt was then cooled to ambient temperature
  2. 2
    workup.WAITleft
  3. 3
    SonstigeA colourless crystalline compound precipitated which
  4. 4
    Sonstigemilted at 174°-178° C
  5. 5
    SonstigeAfter recrystallisation from methanol

Vorschrift

8.5 G of the product obtained in Example 2 (a) was suspended in 25 ml of anhydrous pyridine, and 18.4 g of 3,4,5-trimethoxybenzoyl chloride added slowly under agitation. After being left for one hour at ambient temperature the mixture was heated to 80° C. for a further hour. It was then cooled to ambient temperature, diluted with 50 ml of ethanol and left to stand in a refrigerator. A colourless crystalline compound precipitated which milted at 174°-178° C. After recrystallisation from methanol, the melting point was 180°-183° C. The yield was 11.5 g of pure product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04259332uspto-grants-1981_03