Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 19435007 | HCID 19435007 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19434813 | HCID 19434813 | 52.2% |
Reaction Steps
305 mg (0.779 mmol) of the above 2-(4-amino-3-fluorophenyl)-5-ethoxycarbonylmethylamino-6,8-difluoro-4H-1-benzopyran-4-one was dissolved in 20 mL of ethanol, a 2N aqueous solution of sodium hydroxide was added and the mixture was stirred at 50° C. for 40 minutes. The reaction solution was cooled on ice and the crystals were collected by filtration. The crystals were suspended in water, the suspension was adjusted to pH 2 by addition of hydrochloric acid thereto, and the crystals were collected by filtration again and purified by silica gel column chromatography (chloroform:methanol:acetic acid=90:10:1) to give 148 mg of Compound 140 (yield: 52%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05539112 |
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| Source dataset | uspto-grants-1996_07 |
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| ORD ID | ord-7b8da1bf32f3427095dabd1edbc797d7 |
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| Source note | uspto-grants-1996_07 |
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