반응 #1095854

반응 방정식

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

3-methylpiperidine

→

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

수율 94.0%

용매

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도under reflux condition
3. 3
   농축concentrated
4. 4
   workup.ADDITIONInto the residue was added a saturated ammonium chloride aqueous solution
5. 5
   추출the mixture was extracted with tert-butyl methyl ether three times
6. 6
   세척The organic layers were washed with a saturated sodium chloride aqueous solution
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   농축concentrated

실험 절차

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)).

출처