反应详情

To a stirred solution of 40 g (18 mmol) (4-methoxy-benzooxazol-2-yl)-carbamic acid methyl ester and 4.4 g (54 mmol) sodium acetate in 20 ml acetic acid at room temperature was added dropwise 8.8 g (54 mmol) iodine monochloride and stirring continued for 30 h. The mixture was then poured onto water and extracted three times with ethyl acetate. The combined organic phases were washed with 1 M aqueous sodium thiosulphate solution, then dried over sodium sulfate and concentrated in vacuo. Trituration in ether afforded 4.1 g (65%) (7-iodo-4-methoxy-benzooxazol-2-yl)-carbamic acid methyl ester as a white crystalline solid. ES-MS m/e (%): 349 (M+H+, 100).

1. additionThe mixture was then poured onto water
2. extractionextracted three times with ethyl acetate
3. washThe combined organic phases were washed with 1 M aqueous sodium thiosulphate solution
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo