反应详情

In a 500 ml eggplant-shaped flask equipped with a stirrer, 17.4 g (75.1 mmoles) of 2-chloro-N-(4,6-dimethoxy-5-pyrimidinyl)acetamide was dissolved in 300 ml of dichloromethane, and 5.22 g of benzyl tributyl ammonium chloride was added. Under ice cooling, 41.5 ml of a 50% aqueous solution of sodium hydroxide was added to the mixture with stirring. Thereafter, a solution of 13.8 g (82.6 mmoles) of N-(1-chloroethyl)pyrazole hydrochloride in 70 ml of dichloromethane was added dropwise over about 30 minutes. The mixture was stirred further at room temperature for 2 hours. The reaction mixture was washed with water, dried and concentrated. The resulting solid was recrystallized from isopropanol to give 9.26 g of 2-chloro-N-(4,6-dimethoxy-5-pyrimidinyl)-N-(1-(1-pyrazolyl)ethyl)acetamide as a pale yelllow solid which had the following properties.

1. customIn a 500 ml eggplant-shaped flask equipped with a stirrer
2. stirringThe mixture was stirred further at room temperature for 2 hours
3. washThe reaction mixture was washed with water
4. customdried
5. concentrationconcentrated
6. customThe resulting solid was recrystallized from isopropanol