HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 136396872, compound → HCID 136396995, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 136396872 | HCID 136396872 | — |
| Catalyst | Molybdenum carbonyl (Mo(CO)6) | HCID 98885 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 136396995 | HCID 136396995 | 78% |
Reaction Steps
To a solution of Example 83A (905 mg, 1.6 mmol) in CH3CN (72 mL) and H2O (5 mL) was added molybdenum hexacarbonyl (293 mg, 1.1 mmol) and the solution was refluxed for 2 hours, cooled to room temperature, solvent removed in vacuo and the crude residue purified by column chromatography on silica gel (2% methanol/chloroform) to give the title compound as a colorless solid (670 mg, 78%): 1H NMR (d6-DMSO) δ 14.34 (s, 1H), 9.64 (s, 1H), 8.59 (br s, 2H), 8.13, 8.11 (d, 1H), 7.93 (s, 1H), 7.69-7.45 (m, 4H), 7.27, 7.24 (d, 1H), 2.08-1.95 (m, 1H), 1.92-1.80 (m, 1H), 1.30-0.99 (m, 4H), 0.54-0.46 (m, 1H), 1.50 (s, 9H), 1.45-1.23 (m, 1H), 1.18-0.96 (m, 1H), 0.92-0.62 (m, 7H); MS (ESI) m/z 541 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07517876B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-cf261c2465234c36a29d90e0f55ddc6b |
| Source note | uspto-grants-2009_04 |