反応 #1365694

反応方程式

water

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

terephthaloyl chloride

sodium carbonate

terephthaloyl chloride

→

desired polymer

収率 89.2%

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

収率 89.2%

溶媒

chloroform

ethanol

chloroform

chloroform

chloroform

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.DISSOLUTIONdissolves
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 5 minutes
8. 8
   その他resulting in an emulsion
9. 9
   workup.ADDITIONis added to the flask as quickly as possible
10. 10
    workup.STIRRINGThe reaction mixture is stirred at room temperature and at high speed for 2-3 hours
11. 11
    workup.ADDITIONAt the end of this period the thickened gel-like solution is poured into a 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 dissolves. Then, 7.641 g of 4,4′-diamino-2,2′-biphenyldisulfonic acid (DABS, 85%) is added, and the mixture is stirred until a homogeneous solution is obtained. A solution containing 2.00 g of PEG 200 dioleate surfactant dissolved in 100 ml of purified chloroform is prepared and set aside. Another solution containing 3.806 g of terephthaloyl chloride 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 5 minutes, resulting in an emulsion. Then, the chloroform solution containing the terephthaloyl chloride is added to the flask as quickly as possible. The reaction mixture is stirred at room temperature and at high speed for 2-3 hours. At the end of this period the thickened gel-like solution is poured into a large flask containing 300 ml ethanol/900 ml acetone. The resulting solid is filtered and dried in a vacuum oven to give the desired polymer (9.15 g) as a fluffy light purple solid.

出典