反应详情

A mechanically stirred slurry of 5.00 g of thiophene-3,4-dicarboxylic acid (purchased from Aldrich) in 58.2 mL of 2-methyl-1-propanol was treated with 11.0 mL of chlorotrimethylsilane at room temperature. After completion of the addition, the reaction mixture was stirred at room temperature for 1 h, then at 65° C. for one day, quenched with water at 0° C. and extracted with ether. The combined organic phases were washed with saturated water solution of sodium carbonate, brine, dried over magnesium sulfate, filtered, concentrated on a rotary evaporator, and distilled in vacuum to give 7.86 g (95%) of the title compound of 99.6% GC-purity (bp 113° C./1 mm Hg; colorless oil).

1. additionAfter completion of the addition
2. waitat 65° C. for one day
3. customquenched with water at 0° C.
4. extractionextracted with ether
5. washThe combined organic phases were washed with saturated water solution of sodium carbonate, brine
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated on a rotary evaporator
9. distillationdistilled in vacuum