反应详情

温度

30 °C

A mixture of 3-methyl-5[4-(trifluoromethyl)phenyl]thiophene-2-carboxylic acid (intermediate 130, 8.1 g) in methanol (300 ml) was heated at 30° C. and hydrogen chloride gas bubbled through the mixture. The reaction mixture was then stirred at reflux for 21 hours; cooled and treated with further hydrogen chloride gas. The reaction mixture was stirred at reflux for a further 6 hours, cooled and concentrated. The resulting precipitate was filtered and washed with cyclohexane to give the title compound as a solid.

1. customhydrogen chloride gas bubbled through the mixture
2. temperatureat reflux for 21 hours
3. temperaturecooled
4. additiontreated with further hydrogen chloride gas
5. stirringThe reaction mixture was stirred
6. temperatureat reflux for a further 6 hours
7. temperaturecooled
8. concentrationconcentrated
9. filtrationThe resulting precipitate was filtered
10. washwashed with cyclohexane