反应详情

In 150 ml of methylene chloride was suspended 5.00 g of 2-(2,4-difluorophenylamino)-5-fluoro-6-methoxynicotinic acid, and 5.98 g of thionyl chloride and 3 drops of N,N-dimethylformamide was added thereto, after which the resulting mixture was subjected to reaction under reflux for 2 hours. The solvent and the excessive thionyl chloride were removed by distillation under reduced pressure, and to the crystalline material thus obtained was added 10 ml of n-hexane, after which crystals were collected by filtration to obtain 4.87 g (yield 91.7%) of 2-(2,4-difluorophenylamino)-5-fluoro-6-methoxynicotinoyl chloride having a melting point of 153°-154° C.

1. additionwas added
2. customafter which the resulting mixture was subjected to reaction
3. temperatureunder reflux for 2 hours
4. customThe solvent and the excessive thionyl chloride were removed by distillation under reduced pressure
5. customto the crystalline material thus obtained
6. filtrationafter which crystals were collected by filtration