反应详情

温度

100 °C

To a solution of 1000 mg (3.5 mmol) of 4-(4-chloro-2-methyl-pyrrolo[2,3-d]pyrimidin-7-yl)-butyric acid ethyl ester (example 2a) in 7 ml N-methylpyrrolidone were added 1590 mg (5.4 mmol) of (2S)-3-amino-2-benzyloxycarbonylamino-propionic acid tert-butyl ester and 5.9 ml triethylamine and the reaction was stirred at 100° C. for 36 h. The reaction was diluted with 85 ml EE and extracted with water, aqueous citric acid and again with water. The organic phase was dried over MgSO4 filtered and the solvent was removed in vacuo. The residue was chromatographed on silica gel eluting with DCM/EE (2:1). Yield: 719 mg.

1. additionThe reaction was diluted with 85 ml EE
2. extractionextracted with water, aqueous citric acid and again with water
3. dry with materialThe organic phase was dried over MgSO4
4. filtrationfiltered
5. customthe solvent was removed in vacuo
6. customThe residue was chromatographed on silica gel eluting with DCM/EE (2:1)