HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4,6-Trimethylpyridine → HCID 15153821, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | Methacryloyl chloride | HCID 13528 | — |
| Reactant | 1-Decanol, 10-bromo- | HCID 104507 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15153821 | HCID 15153821 | 70% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
2,4,6-Collidin (12.3 ml, 92.7 mmol, 1.1 eq.) was added to a solution of 10-bromodecanol (20.0 g, 84.3 mmol) in anhydrous dichloromethane (200 ml). After cooling the mixture to 0° C. methacrylic acid chloride (16.5 ml, 168.6 mmol, 2 eq.) was slowly added dropwise and the reaction mixture was stirred for 1 h at 0° C. and at for 15 h room temperature. The reaction mixture was then washed with water (100 ml) and cold 1N HCl (100 ml). The combined organic phases were dried with anhydrous sodium sulphate. After removal of the solvent under reduced pressure the obtained crude product was purified by column chromatography (eluent: hexane/dichloromethane 8:2). 18.0 g (70% yield) of the product was obtained as a colorless liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040602B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-115dfc1246384b20bdc0e7770cb99700 |
| Source note | uspto-grants-2015_05 |