Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 10673123 | HCID 10673123 | — |
| Product | HCID 19434887 | HCID 19434887 | 36% |
Reaction Steps
10 mL of concentrated sulfuric acid was added to 1.00 g (1.98 mmol) of 6,8-difluoro-2-(3-fluoro-4-pivaloylaminophenyl)-7-hydroxymethyl-5-pivaloylamino-4H-1-benzopyran-4-one obtained in Example 118 (4) and the mixture was stirred at 50° C. for 20 minutes. The reaction solution was cooled on ice, ice water was added and the precipitated crystals were collected by filtration. The crystals were purified by silica gel column chromatography (chloroform:methanol=9:1-chloroform:methanol:aqueous ammonia=40:10:1) and triturated with ethanol to give 293 mg of Compound 119 (yield: 36%).
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-e89f4379550e4308989dbf4cd8bb233d |
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| Source note | uspto-grants-1996_07 |
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