反応 #1365695

反応方程式

terephthaloyl chloride

water

terephthaloyl chloride

4,4′-diamino-2,2′-biphenyldisulfonic acid

sodium carbonate

→

desired polymer

収率 89.5%

4,4′-diamino-2,2′-biphenyldisulfonic Acid benzene-1,4-dicarbonyl Chloride

収率 89.5%

溶媒

chloroform

chloroform

chloroform

chloroform

ethanol

反応条件

後処理

1. 1
   その他Into a 1-L fluted round-bottom flask equipped with a mechanical stirring shaft
2. 2
   workup.DISSOLUTIONis dissolved
3. 3
   その他is obtained
4. 4
   その他is prepared
5. 5
   その他is also prepared
6. 6
   workup.STIRRINGThe reaction flask is stirred at high speed (800-1000 rpm)
7. 7
   workup.STIRRINGThe mixture is stirred for five minutes
8. 8
   その他resulting in an emulsion
9. 9
   workup.ADDITIONadded to the flask as quickly as possible
10. 10
    workup.STIRRINGThe reaction mixture is stirred at high speed at room temperature for 2-3 hours
11. 11
    workup.ADDITIONAt the end of this period the thickened gel-like solution is poured into large flask
12. 12
    ろ過The resulting solid is filtered
13. 13
    その他dried in a vacuum oven

実験手順

Into a 1-L fluted round-bottom flask equipped with a mechanical stirring shaft, is placed 250 mL of deionized water and 7.95 g of sodium carbonate. The mixture is stirred until the carbonate salt is dissolved. Then, 7.64 g of 4,4′-diamino-2,2′-biphenyldisulfonic acid (DABS, 85%) is added and stirring is continued until a homogeneous solution is obtained. A solution containing 2.00 g of PEG 400 distearate surfactant dissolved in 100 mL of purified chloroform is prepared and set aside. Another solution containing 3.79 g of terephthaloyl chloride and 0.05 g of 1,5-benzenetricarbonyl trichloride dissolved in 100 mL of purified chloroform is also prepared. The reaction flask is stirred at high speed (800-1000 rpm), and the chloroform/surfactant solution is added quickly to the flask. The mixture is stirred for five minutes, resulting in an emulsion. Then, the chloroform solution containing the terephthaloyl chloride added to the flask as quickly as possible. The reaction mixture is stirred at high speed at room temperature for 2-3 hours. At the end of this period the thickened gel-like solution is poured into large flask containing 300 mL ethanol/900 mL acetone. The resulting solid is filtered and dried in a vacuum oven to provide 9.15 grams of the desired polymer as a fluff, light purple solid.

出典