反应详情

温度

0 °C

With ice cooling, 1.20 g of 4-methoxy-3,5-dimethylbenzoyl chloride, dissolved in 1 ml of dry dichloromethane were initially added dropwise to a solution of 0.82 g of 4,6-dichloropyridin-3-ylamine in 8 ml of dry dichloromethane. A solution of 0.4 ml of absolute pyridine in 1 ml of dry dichloromethane was then added, and the reaction was stirred at 0° C. for 2 h, the product partially precipitating slowly. Approx. 10 ml of 10% strength aqueous sodium bisulfate solution were then added, and the mixture was stirred for five minutes. The aqueous phase was then decanted off and the solid-containing organic phase was concentrated under reduced pressure and freeze-dried. This gave 1.63 g (100%) of the product, which was used for the next step without any further purification.

1. customthe product partially precipitating slowly
2. additionApprox. 10 ml of 10% strength aqueous sodium bisulfate solution were then added
3. stirringthe mixture was stirred for five minutes
4. customThe aqueous phase was then decanted off
5. concentrationthe solid-containing organic phase was concentrated under reduced pressure
6. customfreeze-dried
7. customThis gave 1.63 g (100%) of the product, which was used for the next step without any further purification