反应详情

A 25 ml of two-neck round bottom flask was filled with argon gas and the solution of 4-amino-3-fluoro-benzonitrile (300 mg, 2.204 mmol, 1 equiv.) in methylenechloride was put into the flask. To the solution was added iodomonochloride (393.6 mg, 2.424 mmol, 1.1 equiv.) and stirred for 1 hour. After confirming the completion of the reaction with TLC, to resulting solution was added saturated sodium thiosulphate solution and stirred. The reaction solution was extracted with methylenechloride, washed with water(twice) and brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The obtained liquid was column-chromatographed (n-hexane/ethylacetate=3/1) to yield a brown liquid.

1. additionA 25 ml of two-neck round bottom flask was filled with argon gas
2. customthe completion of the reaction with TLC
3. customto resulting solution
4. stirringstirred
5. extractionThe reaction solution was extracted with methylenechloride
6. washwashed with water(twice) and brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe obtained liquid was column-chromatographed (n-hexane/ethylacetate=3/1)
11. customto yield a brown liquid