Reacción #1365711

Ecuación de reacción

Bis(trimethylsilyl)chloromethane

sodium acrylate

phenothiazine

→

desired product

Bis(trimethylsilyl)methylacrylate

Disolventes

butyronitrile

—

hexanes

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroequipped with a condenser, mechanical stirrer and a nitrogen inlet
2. 2
   Temperaturaheated
3. 3
   Temperaturato reflux
4. 4
   Filtraciónfiltered
5. 5
   Otroto remove the solids
6. 6
   OtroThe solvents were removed under reduced pressure
7. 7
   workup.DISTILLATIONFractional distillation of the residue under reduced pressure

Procedimiento

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.

Fuente