반응 #42815

반응 방정식

3,3-dimethylpyrrolidine

N,N-dimethylformamide

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

potassium carbonate

→

4-(2-butynyloxy)-5-fluoro-6-(3,3-dimethylpyrrolidin-1-yl)pyrimidine

수율 31.7%

용매

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   온도The reaction mixture was cooled to near room temperature
3. 3
   세척the mixture was washed with a saturated sodium chloride aqueous solution three times
4. 4
   건조The organic layers were dried over anhydrous magnesium sulfate
5. 5
   농축concentrated

실험 절차

Into 4 ml of N,N-dimethylformamide was resolved 0.36 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine, 0.62 g of potassium carbonate and 0.25 g of 3,3-dimethylpyrrolidine was added therein, and the mixture was stirred for 6 hours at 80° C. The reaction mixture was cooled to near room temperature, ethyl acetate was added therein, and the mixture was 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 0.15 g of 4-(2-butynyloxy)-5-fluoro-6-(3,3-dimethylpyrrolidin-1-yl)pyrimidine (hereinafter, referred to as Compound (28)).

출처