反应详情

35 mg [0.153 mMols] of 4-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)furan-2-carboxylic acid was dissolved in 1.5 mL of DMF and stirred with 120 mg [0.22 mMols] of PyBOP, 50 μL [46 mg, 0.46 mMols] of N-methylmorpholine, and 50 mg [0.26 mMols] of N-(2,2,2-trifluoroethyl) N-2-cyclopropylethylamine overnight at ambient temperature. The solvent was removed under a nitrogen stream at 30° C. and residue dissolved in methanol with several drops of TFA to protonate the amines present. The crude material was purified via C18 silica utilizing a gradient of water/acetonitrile/TFA as an eluent 5%-95%. The product, 4 mg of a beige powder (after lyophilization of filtrates) was obtained; yield 9.5%.

1. customThe solvent was removed under a nitrogen stream at 30° C.
2. dissolutionresidue dissolved in methanol with several drops of TFA
3. customThe crude material was purified via C18 silica utilizing a gradient of water/acetonitrile/TFA as an eluent 5%-95%