HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 58348421, compound → HCID 58348350, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 58348421 | HCID 58348421 | — |
| Catalyst | HCID 178479819 | HCID 178479819 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58348350 | HCID 58348350 | 80.1% |
Reaction Steps
To 2-but-3-enyl-2-(3-fluoro-phenyl)-hex-5-enoic acid methyl ester (Example 12a) (5.0 g) in dichloromethane (100 mL) was added Grubbs Catalyst (2nd Generation, Sigma-Aldrich Company Ltd) (0.05 g). The mixture was warmed to reflux under nitrogen. After 20 hours the reaction was cooled to room temperature, evaporated to an oil and purified by column chromatography on silica eluting with ethyl acetate/isohexane (5/95) to yield an oil. Analysis of the product showed that significant amounts of starting material was present in the mixture so the mixture was subjected to a repetition of the reaction conditions and purification as above to afford the subtitled compound as a coloured oil (3.60 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08329729B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-d0b5ed7d6bd94bb28f8d69df9db62304 |
| Source note | uspto-grants-2012_12 |