反応 #42819

反応方程式

ammonium chloride

sodium hydride

3,3-dimethylpiperidine hydrochloride

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

→

4-(2-butynyloxy)-6-(3,3-dimethylpiperidino)-5-fluoropyrimidine

収率 18.1%

溶媒

tetrahydrofuran

反応条件

後処理

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

実験手順

0.12 g of sodium hydride (60% oil suspension) was suspended in 2 ml of tetrahydrofuran. 0.18 g of 3,3-dimethylpiperidine hydrochloride and 0.20 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine were added therein, and the mixture was stirred for 1 hour at 60%. After 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 0.05 g of 4-(2-butynyloxy)-6-(3,3-dimethylpiperidino)-5-fluoropyrimidine (hereinafter, referred to as Compound (32)).

出典