반응 #1365710

반응 방정식

2-Trimethylsilylethanol

methacryloyl chloride

pyridine

→

desired product

수율 44.7%

2-Trimethylsilylethylmethacrylate

수율 44.7%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   기타equipped with a condenser, addition funnel, magnetic stirrer and a nitrogen inlet
2. 2
   기타A mildly exothermic reaction
3. 3
   workup.STIRRINGThe mixture was stirred overnight at room temperature
4. 4
   세척Afterwards, the mixture was washed with 1×100 ml
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   농축The solution was concentrated in vacuo
7. 7
   workup.DISTILLATIONFractional distillation under reduced pressure

실험 절차

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.

출처