반응 #1365711

반응 방정식

Bis(trimethylsilyl)chloromethane

sodium acrylate

phenothiazine

→

desired product

Bis(trimethylsilyl)methylacrylate

용매

butyronitrile

—

hexanes

반응 조건

후처리

1. 1
   기타equipped with a condenser, mechanical stirrer and a nitrogen inlet
2. 2
   온도heated
3. 3
   온도to reflux
4. 4
   여과filtered
5. 5
   기타to remove the solids
6. 6
   기타The solvents were removed under reduced pressure
7. 7
   workup.DISTILLATIONFractional distillation of the residue under reduced pressure

실험 절차

Bis(trimethylsilyl)chloromethane (Aldrich) 39 g, 0.2 mole), sodium acrylate (28 g, 0.3 mole), Adogen 464 (Aldrich) (6.96 g), and phenothiazine (0.10 grams) were placed in a round bottom flask equipped with a condenser, mechanical stirrer and a nitrogen inlet. The flask was charged with 100 ml of butyronitrile and heated to reflux while stirring. After 6 hours, the mixture was diluted with 150 ml hexanes and filtered to remove the solids. The solvents were removed under reduced pressure. Fractional distillation of the residue under reduced pressure gave 35.5 grams 975%) of the desired product at 45-58° C. at 0.5 mm pressure.

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