反应详情

The 4-iodo-2-methoxybenzoic acid methyl ester of Step A (2.7 g, 9.24 mmol) was dissolved in tetrahydrofuran (40 mL) and 1 N sodium hydroxide (20 mL, 20 mmol) was added. The reaction mixture was heated at reflux for 3 hours, then cooled and concentrated in vacuo to give an orange oil that was partitioned between ethyl acetate and 2 N hydrochloric acid. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give 2.5 g of title product as a yellow-orange solid, m.p. 144–146° C.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 3 hours
3. temperaturecooled
4. concentrationconcentrated in vacuo
5. customto give an orange oil that
6. customwas partitioned between ethyl acetate and 2 N hydrochloric acid
7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo