HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 11256949, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methacryloyl chloride | HCID 13528 | — |
| Reactant | 2-[1,1,1,3,3,3-Hexamethyl-2-(trimethylsilyl)trisilan-2-yl]ethan-1-ol | HCID 13308122 | — |
| Catalyst | Phenothiazine | HCID 7108 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 11256949 | HCID 11256949 | 63% |
Reaction Steps
Methacryloyl chloride (2.50 grams, 0.024 mole) in 25 ml tetrahydro-furan was added dropwise into a solution of 2-tris(trimethylsilyl) silyl ethanol (6.5 grams, 0.022 mole), pyridine (2.0 grams, 0.025 mole) and 25 mg of phenothiazine in 50 ml tetrahydrofuran at room temperature. Stirred at room temperature for two more hours. The solids were filtered off and the solution was washed with 100 ml brine. The solution was then diluted with 100 ml ether and washed with 5% hydrochloric acid, followed by deionized water, and then with brine. It was dried over anhydrous magnesium sulfate and was concentrated in vacuo. Fractional distillation under reduced pressed gave 5 grams of the product at 105-115° C. at 0.5 mm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | USRE038282E1 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-d5cbeb0a93d6451d95cf286ad45a1f7c |
| Source note | uspto-grants-2003_10 |