反应详情

温度

80 °C

Dissolve 5-(4-chloro-phenyl)-3-(2-hydroxy-ethyl)-thiophene-2-carboxylic acid methyl ester (3.4 g, 11.46 mmol) in toluene (60 mL) and add p-toluenesulfonic acid monohydrate (0.3 g, 1.58 mmol) and heat to 80° C. for one hour. Cool the mixture to room temperature and dilute with ethyl acetate (50 mL). Wash the solution with 1 N NaOH and extract the aqueous portion twice with ethyl acetate. Combine the organic fractions, dry over Na2SO4, filter, and concentrate. Triturate the solid with ether and then filter and dry under vacuum to give 1.3 g (43%) of the title compound. LC-MS/ES m/z (35Cl) 265.0 [M+H]+.

1. temperatureCool the mixture to room temperature
2. washWash the solution with 1 N NaOH
3. extractionextract the aqueous portion twice with ethyl acetate
4. dry with materialdry over Na2SO4
5. filtrationfilter
6. concentrationconcentrate
7. customTriturate the solid with ether
8. filtrationfilter
9. customdry under vacuum