Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Acryloyl chloride | HCID 13140 | — |
| Reactant | HCID 178462376 | HCID 178462376 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178459282 | HCID 178459282 | 108.1% |
Reaction Steps
Acryloyl chloride (9 grams), methyl(α-hydroxyethyl)-cyclopentadienyltricarbonylmanganese (13.1 grams), and triethylamine (10.1 grams) were dissolved in 200 ml dichloromethane under a nitrogen atmosphere. A 0.1 gram sample of N,N-dimethylaminopyridine (DMAP) was added as a catalyst. For 4 days the solution was stirred and protected from light while and a white precipitate slowly formed. The reaction mixture was extracted twice with dilute HCl and the dichloromethane phase was dried with magnesium sulfate. The magnesium sulfate was removed by filtration and the dichloromethane solution was filtered through silica gel to remove a colored impurity. The solution was then rotary evaporated to a yellowish oil that was vacuum dried to give 16.2g (97%) of methyl(α-acryloylethyl)cyclopentadienyl-tricarbonylmanganese as a mixture of 1,2 and 1,3 isomers.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06132860 |
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| Source dataset | uspto-grants-2000_10 |
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| ORD ID | ord-515c15931a464e84bcadbac6b83b6f14 |
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| Source note | uspto-grants-2000_10 |
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