반응 #42810

반응 방정식

ammonium chloride

4-chloro-6-(2-butynyloxy)pyrimidine

potassium carbonate

cis-3,5-dimethylpiperidine hydrochloride

→

4-(2-butynyloxy)-6-(cis-3,5-dimethylpiperidino)pyrimidine

수율 96.2%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도The reaction mixture was cooled to near room temperature
3. 3
   추출the mixture was extracted with tert-buthyl methyl ether three times
4. 4
   세척The organic layers were washed with a saturated sodium chloride aqueous solution three times
5. 5
   건조The organic layers were dried over anhydrous magnesium sulfate
6. 6
   농축concentrated

실험 절차

Into 3 ml of N,N-dimethylformamide was resolved 0.3 g of 4-chloro-6-(2-butynyloxy)pyrimidine, 0.57 g of potassium carbonate and 0.25 g of cis-3,5-dimethylpiperidine hydrochloride was added therein, and the mixture was stirred for 40 minutes at 70° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-buthyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution three times. The organic layers were dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.41 g of 4-(2-butynyloxy)-6-(cis-3,5-dimethylpiperidino)pyrimidine (hereinafter, referred to as Compound (23)).

출처