反应详情

A dried 25 ml two-neck round bottom flask was filled with argon gas and the solution of N-(4-aminomethyl-2-vinyl-phenyl)-methanesulfonamide (51 mg, 0.23 mmol) and 3-(4-t-butyl-phenyl)-acrylic acid (1.2 eq, 0.27 mmol, 55.26 mg) in DMF was put into the flask. To the solution were added triethylamine (2 eq, 0.46 mmol, 64.12 mg) and diethylcyanophosphonate (1.2 eq, 0.27 mmol, 41.88 μl) and stirred for 12 hours. After confirming the completion of the reaction with TLC, the reaction solution was extracted with methylenechloride, washed with water and brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The obtained liquid was column-chromatographed (n-hexane/ethyl acetate=1/1) to yield a white solid (48.4 mg, 43.37%).

1. additionA dried 25 ml two-neck round bottom flask was filled with argon gas
2. customthe completion of the reaction with TLC
3. extractionthe reaction solution was extracted with methylenechloride
4. washwashed with water and brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe obtained liquid was column-chromatographed (n-hexane/ethyl acetate=1/1)