反应详情

温度

0 °C

To a solution of 5-acetylthiophene-2-carboxylic acid (3.24 g, 19.0 mmol) dissolved in a mixture of toluene (50 mL) and methanol (50 mL) cooled to 0° C. was added 2.0 M trimethylsilyldiazomethane in ether (19.0 mL, 38.1 mmol) dropwise. Upon complete addition, the reaction mixture was allowed to warm to room temperature overnight. The reaction was quenched with the addition of acetic acid and the solvent was removed. The residue thus obtained was partitioned between ethyl acetate and saturated aqueous NaHCO3 and upon separation, the organic layer was dried over anhydrous magnesium sulfate and concentrated to afford the desired product (3.49 g, 100%). LC-MS: (FA) ES+ 185)

1. additionUpon complete addition
2. temperatureto warm to room temperature overnight
3. customThe reaction was quenched with the addition of acetic acid
4. customthe solvent was removed
5. customThe residue thus obtained
6. customwas partitioned between ethyl acetate and saturated aqueous NaHCO3 and upon separation
7. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
8. concentrationconcentrated