Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 10673123 | HCID 10673123 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10721996 | HCID 10721996 | 94% |
Reaction Steps
3.30 g (6.55 mmol) of 6,8-difluoro-2-(3-fluoro-4-pivaloylaminophenyl)-7-hydroxymethyl-5-pivaloylamino-4H-1-benzopyran-4-one obtained in Example 118 (4) was dissolved in 70 mL of dimethylformamide, 4.6 mL of triethylamine and 1.0 mL of methanesulfonyl chloride were added under ice-cooling and the mixture was stirred at room temperature for 10 minutes. Water was added to the reaction solution and the mixture was extracted twice with ethyl acetate. The organic layer was washed once with water and once with an aqueous saturated solution of sodium chloride, and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to give 3.57 g of 6,8-difluoro-2-(3-fluoro-4-pivaloylaminophenyl)-7-methanesulfonyloxymethyl-5-pivaloylamino-4H-1-benzopyran-4-one (yield: 94%).
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-80fa9ba1048548d598370452d7f21632 |
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| Source note | uspto-grants-1996_07 |
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