反应详情

温度

60 °C

2-Chloro-N-(5-chloropyridin-2-yl)acetamide (30.68 g) obtained in Reference Example 26(1) is dissolved in N,N-dimethylformamide (500 ml), thereto is added sodium acetate (24.55 g), and the mixture is stirred at 60° C. for 5 hours. The reaction solution is diluted with ethyl acetate, washed successively with water and saturated brine. The solution is dried over magnesium sulfate, treated with activated charcoal, and the filtrate is concentrated under reduced pressure. The resulting residue is suspended in n-hexane and crystals are collected by filtration, washed with n-hexane, and dried to give N-(5-chloropyridin-2-yl)-2-acetoxyacetamide (30.58 g). APCI-MS M/Z:229/231[M+H]+

1. washwashed successively with water and saturated brine
2. dry with materialThe solution is dried over magnesium sulfate
3. additiontreated with activated charcoal
4. concentrationthe filtrate is concentrated under reduced pressure
5. filtrationcrystals are collected by filtration
6. washwashed with n-hexane
7. customdried