反应 #95376

反应方程式

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

thionyl chloride

→

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

溶剂

benzene

反应条件

后处理

1. 1
   workup.ADDITIONTo the solution was added
2. 2
   温度The mixture was refluxed
3. 3
   浓缩the reaction solution was concentrated
4. 4
   workup.ADDITIONTo the concentrate was added n-hexane (5 ml)
5. 5
   其他crystallization of the reaction product
6. 6
   过滤The resulting product was recovered by filtration
7. 7
   洗涤washed with n-hexan
8. 8
   其他dried

实验过程

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).

来源