تفاعل #1365711

ord-3901f3841ab847a79d34516e6d4156e3

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىequipped with a condenser, mechanical stirrer and a nitrogen inlet
  2. 2
    درجة الحرارةheated
  3. 3
    درجة الحرارةto reflux
  4. 4
    ترشيحfiltered
  5. 5
    أخرىto remove the solids
  6. 6
    أخرىThe solvents were removed under reduced pressure
  7. 7
    workup.DISTILLATIONFractional distillation of the residue under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06444408B1uspto-grants-2002_09