反应详情

温度

80 °C

3-Mercaptopropionic acid (84 μl, 0.937 mmol) and cesium carbonate (316 mg, 0.970 mmol) were added to an N,N-dimethylformamide (1.0 ml) solution of 5-(2-amino-6-chloropyrimidin-4-yl)-2,4-dimethyl-N-{3-[(tritylamino)methyl]oxetan-3-ylmethyl}benzamide (119 mg, 0.192 mmol) obtained in Step 2 above. The resulting mixture was stirred at 80° C. for 1.5 hour. The reaction solution was slightly acidified with 1N hydrochloric acid, and the precipitated solid was collected by filtration. The separated solid was washed with water, and then dried under reduced pressure. The resulting crude product was purified by silica gel column chromatography (developing solvent: dichloromethane:methanol=15:1) to yield 3-{2-amino-6-[2,4-dimethyl-5-({3-[(tritylamino)methyl]oxetan-3-ylmethyl}carbamoyl)phenyl]pyrimidin-4-ylsulfanyl}propanoic acid (77 mg) as a white solid material.

1. filtrationthe precipitated solid was collected by filtration
2. washThe separated solid was washed with water
3. customdried under reduced pressure
4. customThe resulting crude product was purified by silica gel column chromatography (developing solvent: dichloromethane:methanol=15:1)