Reaktion #95376

Reaktionsgleichung

6,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carboxylic acid

thionyl chloride

→

6,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carbonyl chloride

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONTo the solution was added
2. 2
   TemperaturThe mixture was refluxed
3. 3
   Einengenthe reaction solution was concentrated
4. 4
   workup.ADDITIONTo the concentrate was added n-hexane (5 ml)
5. 5
   Sonstigecrystallization of the reaction product
6. 6
   FiltrationThe resulting product was recovered by filtration
7. 7
   Waschenwashed with n-hexan
8. 8
   Sonstigedried

Vorschrift

6,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carboxylic acid (57.3 mg) was dissolved in benzene (10 ml). To the solution was added with stirring at room temperature thionyl chloride (0.5 ml). The mixture was refluxed with stirring for three hours, and the reaction solution was concentrated. To the concentrate was added n-hexane (5 ml) to cause crystallization of the reaction product. The resulting product was recovered by filtration and washed with n-hexan and dried. There were thus obtained 34.8 mg of the desired product (34.8 mg).

Quelle