反应详情

Copper(I) chloride (2.5 equivalents) was charged into a reaction container, to which 2-thienyltributyl tin (2.5 equivalents) and 2-iodo-3-diethoxyphosphorylthiophene were added under nitrogen atmosphere while being dissolved in tetrahydrofuran, followed by heating under reflux for 20 hours. After completion of the reaction, the reaction solution was filtered through celite and the resulting residue was washed with ethyl acetate. The filtrate was washed three times with a 1N hydrochloric acid aqueous solution and a 10% saline solution and dried over anhydrous sodium sulfate. The solvent was distilled off, and the resulting crude product was purified with a silica gel column (hexane:ethyl acetate=1:3) to obtain a colorless liquid.

1. additionwere added under nitrogen atmosphere
2. temperatureby heating
3. temperatureunder reflux for 20 hours
4. customAfter completion of the reaction
5. filtrationthe reaction solution was filtered through celite
6. washthe resulting residue was washed with ethyl acetate
7. washThe filtrate was washed three times with a 1N hydrochloric acid aqueous solution
8. dry with materiala 10% saline solution and dried over anhydrous sodium sulfate
9. distillationThe solvent was distilled off
10. customthe resulting crude product was purified with a silica gel column (hexane:ethyl acetate=1:3)
11. customto obtain a colorless liquid