反応 #2408

反応方程式

water

2-(6-chloropyrimidin-4-yloxy)ethanol

sodium azide

→

2-(6-azidopyrimidin-4-yloxy)ethanol

収率 28.9%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   温度After cooling
2. 2
   抽出extracted with ethyl acetate
3. 3
   乾燥The ethyl acetate layer is dried
4. 4
   その他evaporated
5. 5
   その他to remove the solvent
6. 6
   その他The residue is purified by silica gel column chromatography (solvent; hexane/ethyl acetate=1:1)

実験手順

To a solution of 2-(6-chloropyrimidin-4-yloxy)ethanol (5.61 g) in dimethylformamide (60 ml) is added sodium azide (4.18 g), and the mixture is stirred at 70° C. for 20 hours. After cooling, the reaction solution is treated with water, and extracted with ethyl acetate. The ethyl acetate layer is dried, and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; hexane/ethyl acetate=1:1) to give 2-(6-azidopyrimidin-4-yloxy)ethanol (1.68 g).

出典