120800-05-7

基本信息
1-(5,6-二氯吡啶-3-基)乙酮
1-(5,6-DICHLOROPYRIDIN-3-YL)ETHANONE
1-(5,6-Dichloro-3-pyridinyl)ethanone
Ethanone, 1-(5,6-dichloro-3-pyridinyl)-
1-(5,6-Dichloropyridin-3-yl)ethan-1-one
制备方法

162327-73-3

676-58-4

120800-05-7
以5,6-二氯-N-甲氧基-N-甲基吡啶-3-甲酰胺和甲基氯化镁为原料合成1-(5,6-二氯吡啶-3-基)乙酮的一般步骤如下:在0℃及氮气保护下,向搅拌的5,6-二氯-N-甲氧基-N-甲基吡啶-3-甲酰胺的四氢呋喃溶液(100mL)中缓慢滴加3M甲基氯化镁的四氢呋喃溶液(18mL,54.7mmol)。滴加完毕后,保持反应混合物在0℃下继续搅拌1小时。随后,将反应混合物在0℃下用乙醚和饱和氯化铵水溶液进行分配。分离水层,并用乙酸乙酯萃取。合并所有有机相,用盐水洗涤,无水硫酸钠干燥,过滤后减压浓缩。所得残余物通过快速色谱法纯化,采用90:10至70:30的己烷:乙酸乙酯梯度洗脱,最终得到5.92g 1-(5,6-二氯吡啶-3-基)乙酮,为白色固体,两步总收率为85%。
参考文献:
[1] Patent: US2010/120862, 2010, A1. Location in patent: Page/Page column 95-96
[2] Patent: US2010/137306, 2010, A1. Location in patent: Page/Page column 169-170
[3] Patent: US2010/130499, 2010, A1. Location in patent: Page/Page column 124
[4] Patent: WO2008/132600, 2008, A2. Location in patent: Page/Page column 281-282, 306
[5] Patent: WO2008/133973, 2008, A1. Location in patent: Page/Page column 72; 74