反应 #1095854

反应方程式

4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine

3-methylpiperidine

→

4-(2-butynyloxy)-5-fluoro-6-(3-methylpiperidino) pyrimidine

收率 94.0%

溶剂

ethanol

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   温度under reflux condition
3. 3
   浓缩concentrated
4. 4
   workup.ADDITIONInto the residue was added a saturated ammonium chloride aqueous solution
5. 5
   萃取the mixture was extracted with tert-butyl methyl ether three times
6. 6
   洗涤The organic layers were washed with a saturated sodium chloride aqueous solution
7. 7
   干燥dried over anhydrous magnesium sulfate
8. 8
   浓缩concentrated

实验过程

Into 3 ml of ethanol was resolved 0.3 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine, 0.45 g of 3-methylpiperidine was added therein, and the mixture was stirred for 10 hours under reflux condition. The reaction mixture was cooled to near room temperature, and concentrated. Into the residue was added a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.37 g of 4-(2-butynyloxy)-5-fluoro-6-(3-methylpiperidino) pyrimidine (hereinafter, referred to as Compound (3)).

来源