HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 86755997, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 86755995 | HCID 86755995 | — |
| Reactant | HCID 131722135 | HCID 131722135 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 86755997 | HCID 86755997 | 67% |
Reaction Steps
A solution of cis-4-[(3,5-bis-trifluoromethyl-benzyl)-methoxycarbonyl-amino]-6-hydroxy-7-methoxy-2-methyl-3,4-dihydro-2H-quinoline-1-carboxylic acid ethyl ester (30 mg, 0.053 mmol), triphenylphosphine (28 mg, 0.11 mmol), ethanol (16 μL, 0.79 mmol), and bis-(N-methylpiperazinyl)-azodicarboxamide (30 mg, 0.11 mmol) in benzene (1 mL) was stirred at room temperature for 12 hours. Purification of the solution directly by silica gel chromatography using 0-20% ethyl acetate/hexanes as eluent afforded 20 mg of the title compound (67%): MS m/z 593 (M+), 610 (M++17); 1H NMR (CDCl3) δ6.39 (C5, s, 1H), 1.17 (C2-Me, d, 3H, J=6.2 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06362198B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-486d5615dd9b4ab18b0f57e96bf9985b |
| Source note | uspto-grants-2002_03 |