反応 #1810789

反応方程式

3,4-dihexoxythiophene

thiophene

sulfuric acid

thiodiglycolic acid

→

thiodiglycolic acid diethylester

収率 90.0%

溶媒

ethanol

反応条件

後処理

1. 1
   その他to prepare a reaction solution
2. 2
   温度the reaction solution was refluxing
3. 3
   温度under heating for 12 hr
4. 4
   その他Subsequently, substantially 500 mL of water and ethanol was removed from the reaction solution
5. 5
   workup.ADDITIONFurthermore, 400 mL of ethanol was added
6. 6
   温度after refluxing
7. 7
   温度under heating for 20 hr
8. 8
   workup.ADDITIONthe reaction solution was added water
9. 9
   抽出to extract with ether
10. 10
    乾燥A layer of ether was dried with magnesium sulfate
11. 11
    ろ過by filtering
12. 12
    濃縮concentrating
13. 13
    workup.DISTILLATIONThe residue was distilled under reduced pressure of 200 Pa

実験手順

An example of synthesizing 3,4-dihexoxythiophene as a thiophene monomer is shown below. 2 mL of sulfuric acid was added in an ethanol solution (800 mL) of thiodiglycolic acid (250 g, 1.67 mol) to prepare a reaction solution, then the reaction solution was refluxing under heating for 12 hr after stirring for 24 hr. Subsequently, substantially 500 mL of water and ethanol was removed from the reaction solution according to azeotropy. Furthermore, 400 mL of ethanol was added and after refluxing under heating for 20 hr, the reaction solution was added water to extract with ether. A layer of ether was dried with magnesium sulfate, followed by filtering and concentrating. The residue was distilled under reduced pressure of 200 Pa and a temperature of 100 to 110 degree centigrade, and thereby thiodiglycolic acid diethylester was obtained at a yield of 90 percent.

出典