反应详情

A solution of 5-((3,5-dimethoxyphenyl)ethynyl)-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidin-4-amine (4.27 g) obtained in Step 3 in methylene chloride (20 ml) was cooled to 0° C., and TFA 10 ml was added thereto. The reaction mixture was stirred at room temperature for 5 hours, and the solvent was distilled off under reduced pressure. THF (50 ml) was added to the residue, and the mixture was cooled to 0° C. 4N aqueous sodium hydroxide (12.5 ml) was added thereto, and the mixture was stirred at room temperature overnight. The result was extracted with ethyl acetate, and dried over anhydrous magnesium sulfate. Subsequently, the solvent was distilled off under reduced pressure, and chloroform was added to the resulting residue. The mixture was subjected to filtration to obtain the title compound as a white solid (2.60 g). Physical properties: m/z [M+H]+ 295.3

1. distillationthe solvent was distilled off under reduced pressure
2. additionTHF (50 ml) was added to the residue
3. temperaturethe mixture was cooled to 0° C
4. addition4N aqueous sodium hydroxide (12.5 ml) was added
5. stirringthe mixture was stirred at room temperature overnight
6. extractionThe result was extracted with ethyl acetate
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationSubsequently, the solvent was distilled off under reduced pressure, and chloroform
9. additionwas added to the resulting residue
10. filtrationThe mixture was subjected to filtration