Reaktionsgleichung
O=P(Cl)(Cl)Cl.[S:6]1[CH:10]=[CH:9][CH:8]=[C:7]1[C:11]1[S:12][CH:13]=[CH:14][CH:15]=1.[OH-].[Na+].CN([CH:21]=[O:22])C>>[CH:21]([C:10]1[S:6][C:7]([C:11]2[S:12][CH:13]=[CH:14][CH:15]=2)=[CH:8][CH:9]=1)=[O:22]Komponenten
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
250 ml of DMF in 1 liter flask was added 50.2 ml of POCl3 and stirred for 1 hour at 0° C. to form a complex. 83 g of 2,2'-bithiophene was dissolved in 200 ml of DMF and then added into the complex. After the solution was stirred at 10° C. for 0.5 hour, then the temperature was raised to 40° C. and stirred for 20 hours. The orange viscous product was poured into 3 l beaker and crushed ice cubes were added and stirred for 0.5 hour and then neutralized with 600 ml of 10% aqueous NaOH solution. After the solution was extracted with chloroform, washed with water and dried over anhydrous magnesium sulfate, the solvent was removed under reduced pressure and the crude product was purified by column chromatography. 90 g of product was thus obtained and the melting point thereof was 56°-57° C.
Aufarbeitung
- customto form a complex
- additionadded into the complex
- stirringAfter the solution was stirred at 10° C. for 0.5 hour
- temperaturethe temperature was raised to 40° C.
- stirringstirred for 20 hours
- additionThe orange viscous product was poured into 3 l beaker
- customcrushed ice cubes
- additionwere added
- stirringstirred for 0.5 hour
- extractionAfter the solution was extracted with chloroform
- washwashed with water
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was removed under reduced pressure
- customthe crude product was purified by column chromatography
Quellen und Nachweise
- ORD-Eintrag
- ord-dc12915f5cce4978b61d13b207a36596
- Quelldatensatz
- uspto-grants-1998_05
- Patentnummer
- US05747525
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