反应详情

To a stirred and cooled mixture of 28.4 parts of 2-chloro-m-toluoyl chloride, 12.6 parts of thiophene and 80 parts of methylene chloride is added dropwise a mixture of 39 parts of stannic chloride in 40 parts of methylene chloride at 10° C. Upon completion, stirring is continued first for 2 hours at 20° C and further for 3 hours at reflux. The reaction mixture is poured onto a mixture of ice-water and concentrated hydrochloric acid solution. The methylene chloride solution is separated, washed three times with water, dried, filtered and evaporated. The residue is distilled, yielding 2-chloro-m-tolyl 2-thienyl ketone; bp. 197°-199° C at 12 mm. pressure.

1. temperaturecooled
2. additionis added dropwise
3. stirringUpon completion, stirring
4. temperatureat reflux
5. customThe methylene chloride solution is separated
6. washwashed three times with water
7. customdried
8. filtrationfiltered
9. customevaporated
10. distillationThe residue is distilled