Tributyltin Chloride → HCID 59155833, compound

Participants

Reaction Conditions

Reaction Steps

In THF, 1.96 g (8.90 mmols) of 3-(diethoxyphosphoryl)thiophene was dissolved and cooled down to −78° C. Commercially available n-butyl lithium (1.59 M hexane solution, 8.90 mmols) was slowly dropped, followed by stirring for 3 hours at a standing temperature. Thereafter, 3.19 g (9.80 mmols) of commercially available tributylstannyl chloride was dropped and stirred for 1.5 hours. After completion of the reaction, a disodium hydrogen phosphate/sodium dihydrogen phosphate buffer solution, adjusted to pH=7, was added so as 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:hexane=1:2) to obtain the specified substance in the form of a transparent oil at a yield of 4.35 g (yield: 96%). The thus obtained substance was used as it is for reaction in Example 12(3).

Provenance & Evidence