Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 117839662 | HCID 117839662 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 117933014 | HCID 117933014 | 104.1% |
Reaction Steps
To a tetrahydrofuran solution (2.0 ml) of tert-butyl 5-amino-4-(4-fluorophenyl)-5,6-dihydropyridine-1(2H)-carboxylate (100 mg, 0.342 mmol) synthesized in Reference Synthesis Example 202, triethylamine (52.0 μL, 0.374 mmol) and 4-dimethylaminopyridine (2.08 mg, 0.0170 mmol) were added and then acetic anhydride (26.0 μL, 0.374 mmol) was added with stirring at 0° C., followed by stirring the resultant reaction solution at 0° C. for 2 hours. After completion of the reaction, the reaction solution was purified by silica gel column chromatography to obtain the title compound (119 mg, yield 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09403798B2 |
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| Source dataset | uspto-grants-2016_08 |
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| ORD ID | ord-99a9db030e5f4857b8cd3d7b8501f727 |
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| Source note | uspto-grants-2016_08 |
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