Reaction #95376

Reaction equation

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

thionyl chloride

→

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

Solvents

benzene

Conditions

Workup

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

Procedure

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