反应 #1365711
ord-3901f3841ab847a79d34516e6d4156e3
反应方程式
Bis(trimethylsilyl)chloromethane
sodium acrylate
phenothiazine
→
desired product
Bis(trimethylsilyl)methylacrylate
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他equipped with a condenser, mechanical stirrer and a nitrogen inlet
- 2温度heated
- 3温度to reflux
- 4过滤filtered
- 5其他to remove the solids
- 6其他The solvents were removed under reduced pressure
- 7workup.DISTILLATIONFractional distillation of the residue under reduced pressure
实验过程
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.