反応 #1095884

反応方程式

ammonium chloride

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

potassium carbonate

3,4-dimethylpyrrolidine hydrochloride

→

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

収率 76.2%

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度The reaction mixture was cooled to near room temperature
2. 2
   抽出the mixture was extracted with tert-butyl methyl ether three times
3. 3
   洗浄The organic layers were washed with a saturated sodium chloride aqueous solution
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated

実験手順

Into 3 ml of acetonitrile were added 0.20 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine, 0.41 g of potassium carbonate and 0.20 g of 3,4-dimethylpyrrolidine hydrochloride (cis and trans diastereomer mixture), and the mixture was stirred for 7 hours at 80° 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-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 0.20 g of 4-(2-butynyloxy)-6-(3,4-dimethylpyrrolidin-1-yl)-5-fluoropyrimidine (hereinafter, referred to as Compound (36)).

出典