反应详情

In a two-necked round bottomed flask was added 5-tributylstannyl-2,2'-bithiophene (2.04 g), bis(triphenylphosphine)palladium (II) chloride (0.19 g), 3-formyl-2-hydroxymethyl-5-iodo-thiophene (1.0 g) and tetrahydrofuran (20 ml). The reaction mixture was refluxed for 16 hours. Extracted with ethyl acetate, washed with brine, dried over anhydrous magnesium sulfate and concentrated. The residue was separated by silica gel chromatography, eluted with n-hexane/ethyl acetate (9:1→1:1 gradient) to give brownish solid product (0.43 g, 38%), melting point 108°-110° C.

1. temperatureThe reaction mixture was refluxed for 16 hours
2. extractionExtracted with ethyl acetate
3. washwashed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. customThe residue was separated by silica gel chromatography
7. washeluted with n-hexane/ethyl acetate (9:1→1:1 gradient)