Tributyltin Chloride → HCID 59155929, compound

Participants

Reaction Conditions

Reaction Steps

In 25 ml of THF, 0.952 g (1.34 mmols) of the 3,3′,4,4′-tetrakis(diethoxyphosphoryl)-[2,2′]-bithiophene obtained in Example 6(8) or (9) was dissolved, and cooled down to −78° C. Commercially available n-butyl lithium (1.59 M hexane solution, 5.34 mmols) was slowly dropped, followed by stirring for 3 hours at a standing temperature. Thereafter, 1.956 g (6.01 mmols) of commercially available tributylstannyl chloride was dropped and stirred for 4 hours. After completion of the reaction, a disodium hydrogen phosphate/sodium dihydrogen sulfate buffer solution, adjusted to pH=7, was added to complete the reaction, followed by extraction with ethyl acetate. The organic phase was washed with a saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed, and the resulting crude product was purified with a silica gel column (ethyl acetate) to obtain the specified substance in the form of a transparent oil at a yield of 1.174 g (yield: 68%). The thus obtained substance was used as it is for reaction in Example 6(11).

Provenance & Evidence