反应详情

5-Chloro-4-iodo-2-methoxy benzoic acid methyl ester of Step B (3.00 g, 9.19 mmol) and sodium hydroxide (1.10 g, 27.6 mmol) were combined in methanol (92 mL) and the mixture refluxed for 12 hours. The reaction was cooled to room temperature and solvent evaporated. The residue was dissolved in 1 N sodium hydroxide (75 mL), washed with diethyl ether and the organic washings discarded. The aqueous phase was acidified with 2 N hydrochloric acid and extracted with diethyl ether. The combined extracts were dried over anhydrous sodium sulfate, filtered and concentrated to afford the title carboxylic acid (2.64 g) as orange crystals, m.p. 150–151° C.

1. temperaturethe mixture refluxed for 12 hours
2. customsolvent evaporated
3. dissolutionThe residue was dissolved in 1 N sodium hydroxide (75 mL)
4. washwashed with diethyl ether
5. extractionextracted with diethyl ether
6. dry with materialThe combined extracts were dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated