Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86739514 | HCID 86739514 | — |
| Solvent | Propylene Glycol | HCID 1030 | — |
| Product | HCID 20220949 | HCID 20220949 | — |
Reaction Steps
To all of the compound obtained in step (a) above were added 39 g of sodium hydroxide and 120 ml of propylene glycol, and the mixture was stirred at room temperature for 10 minutes. The liquid reaction mixture was made acidic by addition of 6N hydrochloric acid and was extracted with benzene. The extract was washed with water and dried, and the solvent was removed by distillation. The residue was dissolved in 120 ml of pyridine and 0.6 g of copper powder was added to the solution. The mixture was refluxed for 2 hours, and the copper powder was removed by filtration and the solvent was removed by distillation. The residue was dissolved in n-hexane, and the solution was washed with water and dried. The solvent was removed by distillation and the residue was purified by column chromatography using silica gel to obtain 45 g of the intended compound in the form of an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04456603 |
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| Source dataset | uspto-grants-1984_06 |
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| ORD ID | ord-d2a6032cf9684fc297ded0ab4c76abe5 |
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| Source note | uspto-grants-1984_06 |
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