反应详情

A mixture of (4-tert-Butylphenyl)propynoic acid (step 2 of Example 11, 0.16 mmol, 33.0 mg) and N-(4-aminomethyl-2-fluoro-6-vinylphenyl)methanesulfonamide (step 6 of Example 2, 0.19 mmol, 39.20 mg), DEPC (1.2 eq, 0.19 mmol, 29.13 μl), TEA (2 eq, 0.32 mmol, 44.60 μl) in DMF under an Ar atmosphere was stirred at room temperature for 12 h. Upon completion, as determined by TLC, the reaction solution was extracted by EtOAc (150 ml×3) and the organic phase was washed with H2O, dried (Na2SO4), filtered and concentrated. After silica gel column chromatography (n-hexane/EtOAc=2:1), 3-(4-tert-butylphenyl)propynoic acid 3-fluoro-4-methanesulfonylamino-5-vinylbenzylamide (49.5 mg, 0.11 mmol, 72.25%) was isolated.

1. extractionthe reaction solution was extracted by EtOAc (150 ml×3)
2. washthe organic phase was washed with H2O
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated