HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 919855Generated: November 1, 2026
Trifluoroacetic acid → HCID 86714133, compound
https://huagongshe.com/reaction/919855
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | tert-Butyl {2-[(methanesulfonyl)amino]ethyl}carbamate | HCID 47454467 | — |
| Reactant | 1-Benzyl-5-hydroxy-2-oxo-3-phenyl-1,2-dihydro-[1,7]naphthyridine-6-carboxylic acid methyl ester | HCID 68297358 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86714133 | HCID 86714133 | 33.1% |
Reaction Steps
(2-Methanesulfonylamino-ethyl)-carbamic acid tert-butyl ester (94 mg, 0.38 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 (3 mL). NaOMe was added with vigorous stirring until pH was about 8. The resulting mixture was transferred to a microwave vial containing 1-benzyl-5-hydroxy-2-oxo-3-phenyl-1,2-dihydro-[1,7]naphthyridine-6-carboxylic acid methyl ester (38 mg, 0.098 mmol), and the mixture was heated at 140° C. for 6 h in a microwave reactor. The solvent was evaporated, and the residue was partitioned between EtOAc and 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 16 mg of the title compound. MS: (+) m/z 493.32 (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-2ec2533a78134317a5a5f7bca8d61532 |
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| Source note | uspto-grants-2016_03 |
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