反应详情

2-Amino-4-(4-amino-3-chlorophenoxy)pyridine (236 mg) as disclosed in WO 02/32872 was dissolved in tetrahydrofuran (10 ml) under a nitrogen atmosphere, and then triethylamine (0.21 ml) and phenyl chloroformate (0.188 ml) were added dropwise thereto while cooling in an ice bath, followed by raising the temperature gradually to room temperature and stirring overnight. To the reaction mixture were added N,N-dimethylformamide (2 ml) and morpholine (0.5 ml), followed by further stirring for 1 day. The reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated to give a residue, which was then purified by silica gel column chromatography (eluent; ethyl acetate). Fractions containing the target compound were concentrated to give a residue, to which diethyl ether-hexane was added to suspend, followed by evaporating the solvent. The residue was dried in vacuum to provide the titled compound (172 mg, 49%) as white powder.

1. temperaturewhile cooling in an ice bath
2. stirringby further stirring for 1 day
3. customThe reaction mixture was partitioned between ethyl acetate and water
4. washThe organic layer was washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent was evaporated
7. customto give a residue, which
8. customwas then purified by silica gel column chromatography (eluent; ethyl acetate)
9. additionFractions containing the target compound
10. concentrationwere concentrated
11. customto give a residue
12. customby evaporating the solvent
13. customThe residue was dried in vacuum