HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphoric Acid → HCID 21091439, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphoric Acid | HCID 1004 | — |
| Reactant | [(6R,7S)-2-fluoro-6-methyl-8-oxo-9-(2,2,2-trifluoro-ethyl)-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocyclohepten-7-yl]-carbamic acid tert-butyl ester | HCID 67077130 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21091439 | HCID 21091439 | 83.5% |
Reaction Steps
To a solution of 0.50 g (1.27 mmol) [(6R,7S)-2-fluoro-6-methyl-8-oxo-9-(2,2,2-trifluoro-ethyl)-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocyclohepten-7-yl]-carbamic acid tert-butyl ester in 5 ml tetrahydrofurane were added 1.89 g ortho-phosphoric acid. The mixture was stirred at room temperature for 2 days. Extraction with ethylacetate/water and chromatography on silicagel with dichloromethane/methanol 98/2 yielded 0.31 g (83%) (6R,7S)-7-amino-2-fluoro-6-methyl-9-(2,2,2-trifluoro-ethyl)-6,7-dihydro-9H-5-oxa-9-aza-benzocyclohepten-8-one, MS m/e (%): 293.1 (M+H+, 100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07211573B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-2c7fe17cbbf044dd8c8a9f1e2acf6cb4 |
| Source note | uspto-grants-2007_05 |