反应详情

To a solution of (S)-2-((S)-2-amino-2-cyclohexyl-acetyl)-1,2,3,4-tetrahydro-isoquinoline-1-carboxylic acid (2,6-difluoro-phenyl)-amide trifluoroacetate (63.6 mg, 117 μmol, Eq: 1.00), (S)-2-(tert-butoxycarbonyl-methyl-amino)-propionic acid (22.2 mg, 117 μmol, Eq: 1.00), HATU (49.1 mg, 129 μmol, Eq: 1.1) in DMF (500 μL) at 0° C. was added DIEA (45.5 mg, 61.5 μL, 352 μmol, Eq: 3). The reaction was stirred at RT for 1 h diluted with water and extracted with EtOAc. The combined organics were washed with water, brine, dried with MgSO4 and concentrated in vacuo. The crude material was purified by flash chromatography to give ((S)-1-{(S)-1-cyclohexyl-2-[(S)-1-(2,6-difluoro-phenylcarbamoyl)-3,4-dihydro-1H-isoquinolin-2-yl]-2-oxo-ethylcarbamoyl}-ethyl)-methyl-carbamic acid tert-butyl ester (58 mg) as a white foam.

1. extractionextracted with EtOAc
2. washThe combined organics were washed with water, brine
3. dry with materialdried with MgSO4
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by flash chromatography