反応 #548887

反応方程式

aluminum chloride

2-methylthiophene

p-fluorobenzoyl chloride

hydrochloric acid

→

p-fluorophenyl 5-methyl-2-thienyl ketone

溶媒

water

methylene chloride

反応条件

後処理

1. 1
   その他at 20° C
2. 2
   workup.ADDITIONThe reaction mixture is poured
3. 3
   workup.STIRRINGwhile stirring vigorously
4. 4
   その他The layers are separated
5. 5
   洗浄the aqueous phase is washed with chloroform
6. 6
   その他The organic layers are dried
7. 7
   その他evaporated
8. 8
   その他the latter is evaporated again
9. 9
   その他on triturating in petroleumether
10. 10
    ろ過The solid product is filtered off
11. 11
    その他crystallized from ethanol at -20° C

実験手順

To a stirred mixture of 29.5 parts of 2-methylthiophene, 39.65 parts of p-fluorobenzoyl chloride and 280 parts of methylene chloride are added portionwise 40 parts of aluminum chloride while keeping the temperature at 20° C (water-bath). Upon completion, stirring is continued for 4 hours at room temperature. The reaction mixture is poured onto crushed ice and 50 parts of hydrochloric acid, while stirring vigorously. The layers are separated and the aqueous phase is washed with chloroform. The organic layers are dried and evaporated. The residue is taken up in benzene and the latter is evaporated again. The residue solidifies on triturating in petroleumether. The solid product is filtered off and crystallized from ethanol at -20° C, yielding p-fluorophenyl 5-methyl-2-thienyl ketone; mp. 68° C.

出典