Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 19348360 | HCID 19348360 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 19348329 | HCID 19348329 | 17% |
Reaction Steps
A portion (1.0 g) of the compound obtained in Example 168 was dissolved in acetic acid (30 ml) and to the solution was added 50% sulfuric acid (60 ml). The mixture was stirred for 2 hours at 120° C. and allowed to cool. The reaction mixture was neutralized with 6N aqueous solution of sodium hydroxide and the insoluble matter was filtered off. The filtrate was extracted three times with ethyl acetate, washed with saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was crystallized from ether to yield 170 mg (17%) of the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06040331 |
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| Source dataset | uspto-grants-2000_03 |
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| ORD ID | ord-2b5bdf664c0040d5a2023c8b9cd1a209 |
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| Source note | uspto-grants-2000_03 |
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