反应详情

温度

90 °C

A mixture of 3-chloro-2-formylaminomethyl-isonicotinic acid methyl ester (1.5 g, 6.6 mmol) and phosphorous oxychloride (1.3 mL, 14.2 mmol) in toluene (80 mL) was stirred at 90° C. for 15 minutes, then cooled to room temperature and concentrated under reduced pressure. The residue was partitioned between ethyl acetate and a saturated solution of sodium bicarbonate. The organic layer was separated and washed with water and brine, dried (Na2SO4), filtered and concentrated to give the title compound as a pale yellow solid (1.3 g, 93%). LCMS (method B): RT=2.38 min, [M+H]+=211.

1. temperaturecooled to room temperature
2. concentrationconcentrated under reduced pressure
3. customThe residue was partitioned between ethyl acetate
4. customThe organic layer was separated
5. washwashed with water and brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated