Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Carbon Tetrachloride | HCID 5943 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 23369638 | HCID 23369638 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 23369675 | HCID 23369675 | 95.9% |
Reaction Steps
5-Hydroxy-6-(2-hydroxy-1-vinylethyl)-8methylcarbostyril (7.2 g) was dissolved in pyridine (50 ml), to which triphenylphosphine (25.0 g) and carbon tetrachloride (15 ml) were added in this order, followed by stirring at 60° C. for 3 hours. Methanol (50 ml) was added thereto and stirred for 1 hour. The reaction mixture was filtered. The filtrate was condensed under reduced pressure, to which 1N-HCl was added. Extraction was performed with chloroform. The chloroform phase was dried, and the solvent was evaporated. The residue was recrystallized from a solvent mixture of chloroform-ethyl acetate-ether to obtain 6.4 g of 5-methyl-2,3,6,7-tetrahydro-3-vinylfuro[2,3-f]quinoline-7-one as colorless powdery crystals (95.9%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05576324 |
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| Source dataset | uspto-grants-1996_11 |
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| ORD ID | ord-ad58cdeedd714159bac65ecf8a696c76 |
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| Source note | uspto-grants-1996_11 |
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