反応 #1365710

反応方程式

2-Trimethylsilylethanol

methacryloyl chloride

pyridine

→

desired product

収率 44.7%

2-Trimethylsilylethylmethacrylate

収率 44.7%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

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

実験手順

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.

出典