反応 #1095854

反応方程式

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

3-methylpiperidine

→

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

収率 94.0%

溶媒

ethanol

反応条件

後処理

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

実験手順

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)).

出典