Hydrochloric Acid → 3'',4''-Bis(diethoxyphosphoryl)-[2,2';5',2'';5'',2''';5''',2'''']-quinquethiophene

Participants

Reaction Conditions

Reaction Steps

2,5-bis(tributylstannyl)-3,4-bis(diethoxyphosphoryl)-thiophene and commercially available copper(I) cyanide (2.2 equivalents) were dissolved in solvents indicated in the following Table 11, to which 2-iodobithiophene (2.2 equivalents) was added at room temperature. Thereafter, the reaction mixture was heated to 70° C. and stirred for 4 to 22 hours. After the reaction, the reaction mixture was cooled down to room temperature, to which a 0.6M hydrochloric acid aqueous solution was added, followed by extraction of the resulting product with ethyl acetate. The organic phase was washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed by distilling off under reduced pressure, and the resulting product was purified with a silica gel column (ethyl acetate:methanol=15:1) to obtain the specified substance 1.

Provenance & Evidence