反应 #1365711

ord-3901f3841ab847a79d34516e6d4156e3

反应方程式

C[Si](C)(C)C(Cl)[Si](C)(C)C
Bis(trimethylsilyl)chloromethane
C=CC(=O)[O-].[Na+]
sodium acrylate
c1ccc2c(c1)Nc1ccccc1S2
phenothiazine
C=CC(=O)OC([Si](C)(C)C)[Si](C)(C)C
desired product
C=CC(=O)OC([Si](C)(C)C)[Si](C)(C)C
Bis(trimethylsilyl)methylacrylate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他equipped with a condenser, mechanical stirrer and a nitrogen inlet
  2. 2
    温度heated
  3. 3
    温度to reflux
  4. 4
    过滤filtered
  5. 5
    其他to remove the solids
  6. 6
    其他The solvents were removed under reduced pressure
  7. 7
    workup.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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06444408B1uspto-grants-2002_09