反应详情

After adding a solution of 1-methyl-4-methylaminopiperidine (0.355 ml) in N,N-dimethylformamide (2.5 ml) to crude phenyl N-[6-(4-benzyloxycarbonylamino-3-fluorophenoxy)pyrimidin-4-yl]-N-(phenoxycarbonyl)carbamate (358 mg) at room temperature, the mixture was stirred for 2 hours. The reaction mixture was partitioned between ethyl acetate and water. The separated organic layer was washed with 1N aqueous sodium hydroxide and brine in that order and then dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent; ethyl acetate, then ethyl acetate:methanol=95:5) to provide the title compound (189.4 mg) as white powder.

1. customThe reaction mixture was partitioned between ethyl acetate and water
2. washThe separated organic layer was washed with 1N aqueous sodium hydroxide and brine in that order
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvent was distilled off
5. customthe residue was purified by silica gel column chromatography (Fuji Silysia NH, eluent