Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Potassium bisulfate | HCID 516920 | — |
| Reactant | HCID 10514571 | HCID 10514571 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 10517454 | HCID 10517454 | 80% |
Reaction Steps
The compound prepared in Example B1 (in the general formula (II), R3=H, R4=CH3, and R5=H) (50 mg, 0.20 mmol) was dissolved in pyridine (5 ml), acetyl chloride (80 mg, 0.70 mmol) was added thereto, and the mixture was stirred at 25° C. for one hr. A 15% aqueous potassium hydrogensulfate solution was added to the reaction solution, followed by extraction with methylene chloride. The organic layer was washed with saturated saline and dried over magnesium sulfate, and the solvent was removed by distillation under reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1) to give the title compound (55 mg, 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06255339B1 |
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| Source dataset | uspto-grants-2001_07 |
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| ORD ID | ord-f35c0377f91243f1a1e5a65a099dcd23 |
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| Source note | uspto-grants-2001_07 |
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