反应详情

tert-Butyl 4-(((4-(4-amino-3-fluorophenoxy)-6-cyano-7-quinolyl)oxy)methyl)-1-piperidinecarboxylate (523 mg), pyridine (0.17 ml) and tetrahydrofuran (10 ml) were stirred while cooling on ice, and then phenyl chloroformate was added dropwise. Immediately after completion of the dropwise addition, the cooling bath was removed and the mixture was returned to room temperature. After 15 minutes of stirring, water and ethyl acetate were added for extraction. Silica gel was added to the extract and the solvent was distilled off under reduced pressure for adsorption. The reaction solution-adsorbed silica gel was purified by column chromatography (hexane:ethylacetate=1:1, followed by 1:2, ethyl acetate) in a dry column packed with silica gel, to obtain 490 mg of a yellow powder.

1. temperaturewhile cooling on ice
2. additionImmediately after completion of the dropwise addition
3. customthe cooling bath was removed
4. customwas returned to room temperature
5. additionwater and ethyl acetate were added for extraction
6. additionSilica gel was added to the
7. extractionextract
8. distillationthe solvent was distilled off under reduced pressure for adsorption
9. customThe reaction solution-adsorbed silica gel
10. customwas purified by column chromatography (hexane:ethylacetate=1:1, followed by 1:2, ethyl acetate) in a dry column