HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 919818Generated: November 1, 2026
Trifluoroacetic acid → HCID 86714126, compound
https://huagongshe.com/reaction/919818
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | tert-Butyl {2-[(methanesulfonyl)amino]ethyl}carbamate | HCID 47454467 | — |
| Reactant | 7-Benzyl-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester | HCID 68297735 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86714126 | HCID 86714126 | 59.3% |
Reaction Steps
(2-Methanesulfonylamino-ethyl)-carbamic acid tert-butyl ester (77 mg, 0.32 mmol) was dissolved in CH2Cl2 (2 mL). Trifluoroacetic acid (1 mL) was added, and the mixture was stirred at r.t. for 2 h. Solvent and excess TFA were removed by evaporation, and the residue was taken up in EtOH (2 mL). NaOMe was added with vigorous stirring until pH about 8. The resulting cloudy solution was transferred to a microwave vial containing 7-benzyl-4-hydroxy-8-oxo-7,8-dihydro-[2,7]naphthyridine-3-carboxylic acid methyl ester (25 mg, 0.081 mmol), and the mixture was heated at 140° C. for 6 h in a microwave reactor. The mixture was diluted with EtOAc and washed with 0.1 M HCl. The organic layer was dried over MgSO4 and concentrated. The crude product was purified by silica gel chromatography (0-5% MeOH/CH2Cl2) to give 20 mg of the title compound as an off-white solid. MS: (+) m/z 417.30 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09271970B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-d053dd8d455f4d92a3c443a29898fbe5 |
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| Source note | uspto-grants-2016_03 |
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