反应详情

温度

100 °C

To 20 mL dry methylsulfoxide was added sequentially 7-chloro-3-(3,5-dimethylphenyl)-4-hydroxy-6-iodo-1H-quinolin-2-one (EXAMPLE 4.2 Step B, 1.0 g), 4-dimethylaminopyridine (860 mg), 4-aminopyrimidine (90 mg), [1,1'-bis(diphenylphosphino)ferrocene)-dichloropalladium (II) and the mixture heated to 100° C. under an atmosphere of carbon monoxide. After 72 hours, the mixture was cooled to room temperature and poured into 200 mL ice/water. The pH of the resulting solution was adjusted to pH4 by the addition of acetic acid. The resulting solids were collected by filtration and then re-purified by flash chromatography on silica gel (chlorofonm:methanol, 95:5) to give the title compound (400 mg).

1. temperaturethe mixture was cooled to room temperature
2. filtrationThe resulting solids were collected by filtration
3. customre-purified by flash chromatography on silica gel (chlorofonm:methanol, 95:5)