反应详情

To a solution of 5-isopropoxy-2-amino-benzoic acid (806 mg) in DMF (10 mL) was added 60% in oil NaH (182 mg, 4.53 mmol) at 0-5° C. under an argon atmosphere. The ice bath was removed and the mixture was stirred for 40 min at room temperature. After addition of methyl iodide (0.33 mL, 5.45 mmol) the mixture was stirred at room temperature for an additional 6 h. 10% KHSO4/Na2SO4 was added and the mixture was extracted, washed with brine, dried (Na2SO4), and concentrated to dryness. Purification by chromatography gave 114 mg of 5-isopropoxy-2-amino-benzoic acid methyl ester.

1. customThe ice bath was removed
2. stirringwas stirred at room temperature for an additional 6 h
3. extractionthe mixture was extracted
4. washwashed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated to dryness
7. customPurification by chromatography