反応 #64096

反応方程式

sodium hydride

chloromethyl ethyl ether

2-(4,6-dimethoxypyrimidin-2-yl)-3-methyl-N-methylsulfonylbutyric acid amide

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aimed product

2-(4,6-dimethoxypyrimidin-2-yl)-N-methoxymethyl-3-methyl-N-methylsulfonylbutyric acid amide

溶媒

DMF

反応条件

後処理

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 2 hours
2. 2
   抽出was extracted with 200 ml of diethyl ether
3. 3
   乾燥by drying with anhydrous sodium sulfate
4. 4
   ろ過After filtrating the inorganic salt
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure
6. 6
   その他An only product thus obtained
7. 7
   その他was purified by silica gel column chromatography (developing solvent: N-hexane/ethyl acetate=10/1)

実験手順

2.0 of 2-(4,6-dimethoxypyrimidin-2-yl)-3-methyl-N-methylsulfonylbutyric acid amide was placed in a round bottom flask, and was dissolved in 50 ml of DMF. To the resultant solution, was gradually added 0.28 g of 60% sodium hydride, and the mixture was stirred at room temperature for one hour. Thereafter, 1.0 g of chloromethyl ethyl ether was added dropwise to the resultant mixture, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was then poured into ice water, and was extracted with 200 ml of diethyl ether, followed by drying with anhydrous sodium sulfate. After filtrating the inorganic salt, the solvent was distilled off under reduced pressure. An only product thus obtained was purified by silica gel column chromatography (developing solvent: N-hexane/ethyl acetate=10/1) to obtain 1.8 g of the aimed product of colorless transparent viscous liquid (yield=78.3%) having a refractive index (n20/D) of 1.4976.

出典