反応 #1095875

反応方程式

3-trifluoromethylpiperidine

N,N-dimethylformamide

4-(2-butynyloxy)-5-fluoro-6-chloropyrimidine

potassium carbonate

→

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

収率 108.6%

溶媒

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度The reaction mixture was cooled to near room temperature
3. 3
   洗浄the mixture was washed with a saturated sodium chloride aqueous solution three times
4. 4
   乾燥The organic layers were dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated

実験手順

Into 2 ml of N,N-dimethylformamide was resolved 0.2 g of 4-(2-butynyloxy)-5-fluoro-6-chloropyrimidine, 0.28 g of potassium carbonate and 0.15 g of 3-trifluoromethylpiperidine was added therein, and the mixture was stirred for 5 hours at 70° 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 0.28 g of 4-(2-butynyloxy)-5-fluoro-6-(3-methylpiperidino)pyrimidine (hereinafter, referred to as Compound (26)).

出典