HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 59207311, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methacryloyl chloride | HCID 13528 | — |
| Reactant | HCID 59207328 | HCID 59207328 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59207311 | HCID 59207311 | 86% |
Reaction Steps
Triethylamine (2.10 g, 20.8 mmol) is added dropwise to a solution of 6-(5-bromothiophen-2-yl)methoxyhexanol (3.10 g, 10.62 mmol) and methacryloyl chloride (1.20 g, 11.54 mmol) in DCM (30 mL) at −10° C. This mixture is allowed to warm to room temperature and stirred overnight before it is quenched by the addition water (50 mL) The organic layer is separated and the liquid phase is extracted with DCM (2×30 mL). The organic layers is combined, washed with brine (50 mL), dried (Na2SO4) and evaporated under reduced pressure. The product is purified by column chromatography on silica, eluting with petroleum ether (40-60° C.)/ethyl acetate (90:10) to afford the product as a pale yellow oil (3.27 g, 86%). NMR and MS showed the expected signals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07674397B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-db4847fe29be4bbf9a4b996fd95feb99 |
| Source note | uspto-grants-2010_03 |