反应 #1365710

反应方程式

2-Trimethylsilylethanol

methacryloyl chloride

pyridine

→

desired product

收率 44.7%

2-Trimethylsilylethylmethacrylate

收率 44.7%

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   其他equipped with a condenser, addition funnel, magnetic stirrer and a nitrogen inlet
2. 2
   其他A mildly exothermic reaction
3. 3
   workup.STIRRINGThe mixture was stirred overnight at room temperature
4. 4
   洗涤Afterwards, the mixture was washed with 1×100 ml
5. 5
   干燥dried over anhydrous magnesium sulfate
6. 6
   浓缩The solution was concentrated in vacuo
7. 7
   workup.DISTILLATIONFractional distillation under reduced pressure

实验过程

2-Trimethylsilylethanol (Aldrich) (30 g, 0.25 mole) was placed in a round bottom flask equipped with a condenser, addition funnel, magnetic stirrer and a nitrogen inlet. 200 ml dichloromethane, pyridine (20.80 g, 0.26 mole) and 100 mg of phenothiazine were added to the flask. While stirring, methacryloyl chloride (27.18 g, 0.26 mole) in 100 ml dichloromethane was added dropwise at room temperature. A mildly exothermic reaction occurred. The mixture was stirred overnight at room temperature. Afterwards, the mixture was washed with 1×100 ml deionized water and 2×100 ml brine and dried over anhydrous magnesium sulfate. The solution was concentrated in vacuo. Fractional distillation under reduced pressure gave 20.82 grams of the desired product at 35-38° C. at 0.5 mm.

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