反応 #95376

反応方程式

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

thionyl chloride

→

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

溶媒

benzene

反応条件

後処理

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

実験手順

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).

出典