反应详情

温度

70 °C

(3-Methyl-4-methylsulfanyl-phenyl)-acetic acid (prepared as in PCT WO 2004/052869 A1, Example 57, 1.50 g, 7.64 mmol) was placed in a pressure bottle with methanol (15 mL) and concentrated sulfuric acid (9 drops) and heated at 70° C. for 16 h and then stirred at 25° C. for 2 days. The reaction was then diluted with chloroform and concentrated with silica gel (4 g) in vacuo and purified on Biotage Flash chromatography system (40M column, silica gel, 20% ethyl acetate/hexanes) to afford (3-methyl-4-methylsulfanyl-phenyl)-acetic acid methyl ester (1.34 g, 83%) as an amber oil.

1. concentrationconcentrated with silica gel (4 g) in vacuo
2. custompurified on Biotage Flash chromatography system (40M column, silica gel, 20% ethyl acetate/hexanes)