反应 #64096

反应方程式

sodium hydride

chloromethyl ethyl ether

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

→

aimed product

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

溶剂

DMF

反应条件

后处理

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

实验过程

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.

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