HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phenothiazine → Bis(trimethylsilyl)methylacrylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phenothiazine | HCID 7108 | — |
| Edukt | Bis(trimethylsilyl)chloromethane | HCID 552583 | — |
| Edukt | Sodium acrylate | HCID 4068533 | — |
| Katalysator | Trioctylmethylammonium chloride | HCID 21218 | — |
| Lösungsmittel | Butyronitrile | HCID 8008 | — |
| Produkt | Bis(trimethylsilyl)methylacrylate | HCID 18764809 | — |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06653048B2 |
| Quelldatensatz | uspto-grants-2003_11 |
| ORD ID | ord-0e546afac53e4a3297d14375b599b8ea |
| Quellennotiz | uspto-grants-2003_11 |