反应详情

温度

0 °C

40 g of aluminum chloride and 280 ml of carbon disulfide were taken into a flask, cooled with an ice-salt bath to 0° C. or lower and stirred. A solution of 70 g of 4-bromo-2-fluorobiphenyl as dissolved in 180 ml of carbon disulfide was dropwise added thereto. A solution of 26 g of propionic acid chloride as dissolved in 100 ml of carbon disulfide was dropwise added thereto at 0° C. or lower. After addition, the whole was stirred for 2 hours at 0° C. or lower and then at room temperature overnight. After reaction, the reaction solution was poured into 30 ml of concentrated hydrochloric acid and 300 g of ice and extracted with chloroform. The organic layer was washed three times with water, two times with an aqueous 2% sodium hydroxide solution and then three times with water, and chloroform and carbon disulfide were removed by distillation. The residue was recrystallized from a mixed solvent comprising acetone and methanol to obtain 29 g of 2-fluoro-4-bromo-4'-propionylbiphenyl.

1. additionwas dropwise added
2. additionwas dropwise added
3. customat 0° C.
4. additionAfter addition
5. stirringthe whole was stirred for 2 hours at 0° C.
6. customat room temperature
7. customovernight
8. customAfter reaction
9. extractionextracted with chloroform
10. washThe organic layer was washed three times with water, two times with an aqueous 2% sodium hydroxide solution
11. customthree times with water, and chloroform and carbon disulfide were removed by distillation
12. customThe residue was recrystallized from a mixed solvent comprising acetone and methanol