Réaction #95376

Équation de réaction

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

thionyl chloride

→

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

Solvants

benzene

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONTo the solution was added
2. 2
   TempératureThe mixture was refluxed
3. 3
   Concentrationthe reaction solution was concentrated
4. 4
   workup.ADDITIONTo the concentrate was added n-hexane (5 ml)
5. 5
   Autrecrystallization of the reaction product
6. 6
   FiltrationThe resulting product was recovered by filtration
7. 7
   Lavagewashed with n-hexan
8. 8
   Autredried

Mode opératoire

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).

Source