تفاعل #1365710

معادلة التفاعل

2-Trimethylsilylethanol

methacryloyl chloride

pyridine

→

desired product

المردود 44.7%

2-Trimethylsilylethylmethacrylate

المردود 44.7%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر