反应详情

A mixture of methyl 4-(3-thienylmethoxy)-2-(2-trimethylsilylethoxy)methoxybenzoate (12.1 g) and aqueous potassium carbonate solution (50 mL; 10% w/v) in methanol (200 mL) is heated at reflux for 7 hours. It is then concentrated in vacuo and the residue is treated with water (200 mL) and acidified to pH 1 by treatment with hydrochloric acid (1 N), and the resulting solid is quickly filtered off and is then washed with water. The white solid is then azeotroped with cyclohexane in a Dean-Stark apparatus until no more water is removed. The solid is filtered off, to give 4-(3-thienylmethoxy)-2-(2-trimethylsilylethoxy)methoxybenzoic acid (6.03 g), in the form of a white solid.

1. temperatureis heated
2. temperatureat reflux for 7 hours
3. concentrationIt is then concentrated in vacuo
4. additionthe residue is treated with water (200 mL)
5. filtrationthe resulting solid is quickly filtered off
6. washis then washed with water
7. customThe white solid is then azeotroped with cyclohexane in a Dean-Stark apparatus until no more water
8. customis removed
9. filtrationThe solid is filtered off