Reaktion #215390
ord-b1c815612f6b4507bd14234b027a76db
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturIt was then cooled to ambient temperature
- 2workup.WAITleft
- 3SonstigeA colourless crystalline compound precipitated which
- 4Sonstigemilted at 174°-178° C
- 5SonstigeAfter 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.