反応 #42847

反応方程式

ammonium chloride

4,6-dichloropyrimidine

potassium carbonate

2,5-dimethylhexahydro-1H-azepine hydrochloride

→

1-(6-chloropyrimidin-4-yl)-2,5-dimethylhexahydro-1H-azepine

収率 93.2%

溶媒

acetonitrile

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

Into 3 ml of acetonitrile were added 0.2 g of 4,6-dichloropyrimidine, 0.56 g of potassium carbonate and 0.26 g of 2,5-dimethylhexahydro-1H-azepine hydrochloride, and the mixture was stirred for 3 hours at 80%. 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 0.3 g of 1-(6-chloropyrimidin-4-yl)-2,5-dimethylhexahydro-1H-azepine.

出典