HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 68772134, compound → HCID 68774314, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 68772134 | HCID 68772134 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic acid methanol | HCID 10129899 | — |
| Product | HCID 68774314 | HCID 68774314 | 89.4% |
Reaction Steps
To a solution of Example 11B (60 mg, 0.136 mmol) in mixture of methanol/acetic acid (0.5 mL/0.5 mL), Zn powder (89 mg, 1.36 mmol) was added at room temperature. The reaction mixture was stirred for thirty minutes, filtered, concentrated under reduced pressure and purified by high pressure liquid chromotography (eluting with 0-70% acetonitrile/water and 0.1% trifluoroacetic acid) to provide the title compound (50 mg, 89%). 1H NMR (400 MHz, DMSO-d6) δ ppm 7.85-8.03 (m, 3H), 7.66 (s, 1H), 7.46-7.61 (m, 2H), 5.97-6.16 (m, 1H), 4.02-4.22 (m, 2H), 3.65-3.95 (m, 3H), 2.82-3.04 (m, 2H), 1.68-2.69 (m, 13H), 1.12-1.29 (m, 3H). MS (ESI) m/z 411 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834012B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-baf57315eb644ca9b31253a21d888527 |
| Source note | uspto-grants-2010_11 |