反応 #1365711

反応方程式

Bis(trimethylsilyl)chloromethane

sodium acrylate

phenothiazine

→

desired product

Bis(trimethylsilyl)methylacrylate

溶媒

butyronitrile

—

hexanes

反応条件

後処理

1. 1
   その他equipped with a condenser, mechanical stirrer and a nitrogen inlet
2. 2
   温度heated
3. 3
   温度to reflux
4. 4
   ろ過filtered
5. 5
   その他to remove the solids
6. 6
   その他The solvents were removed under reduced pressure
7. 7
   workup.DISTILLATIONFractional distillation of the residue under reduced pressure

実験手順

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.

出典