反应详情

To a cold (0° C.) solution of 5-[2-amino-6-{2-(cyclopropylmethoxy)-6-[(4-methoxybenzyl)oxy]phenyl}-3-(hydroxymethyl)-4-pyridinyl]-2-(ethylamino)phenol (0.150 g, 0.28 mmol) in THF (5.0 mL) including triethylamine (0.12 mL, 0.83 mmol) was added triphosgene (0.099 g, 0.33 mmol). After being stirred for 30 minutes, the mixture was allowed to warm to room temperature, and the stirring was continued overnight. The resulting mixture was quenched with water and extracted with ethyl acetate. The separated organic phase was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (dichloromethane:methanol, 9:1) to give 7-{2-(cyclopropylmethoxy)-6-[(4-methoxybenzyl)oxy]phenyl}-5-(3-ethyl-2-oxo-2,3-dihydro-1,3-benzoxazol-6-yl)-1,4-dihydro-2H-pyrido[2,3-d][1,3]oxazin-2-one. (0.049 g, 30%); LC-MS (m/z=594, M+1)

1. waitthe stirring was continued overnight
2. customThe resulting mixture was quenched with water
3. extractionextracted with ethyl acetate
4. washThe separated organic phase was washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by column chromatography on silica gel (dichloromethane:methanol, 9:1)