反応 #42842

反応方程式

ammonium chloride

4,6-dichloro-5-methylpyrimidine

sodium hydride

2-butyn-1-ol

→

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

収率 91.2%

溶媒

tetrahydrofuran

tetrahydrofuran

tetrahydrofuran

反応条件

後処理

1. 1
   workup.STIRRINGstirred for 2 hours
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 water
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated

実験手順

0.32 g of sodium hydride (60% oil suspension) was suspended in 12 ml of tetrahydrofuran. 2 ml of tetrahydrofuran solution of 0.43 g of 2-butyn-1-ol was added dropwise at room temperature therein slowly, and the mixture was stirred for 20 minutes. Into the mixture was added dropwise 2 ml of tetrahydrofuran solution of 1 g of 4,6-dichloro-5-methylpyrimidine at 0° C. slowly, and stirred for 2 hours. The reaction mixture was poured into a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with water, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 1.1 g of 4-chloro-6-(2-butynyloxy)-5-methylpyrimidine.

出典