HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 131728427, compound → HCID 131728426, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 131728427 | HCID 131728427 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic acid methanol | HCID 10129899 | — |
| Product | HCID 131728426 | HCID 131728426 | 79% |
Reaction Steps
To a solution of Example 18A (100 mg, 0.24 mmol) in a mixture of methanol/acetic acid (1.0 mL/1.0 mL), Zn powder (170 mg, 2.6 mmol) was added at room temperature. The reaction mixture was stirred for 30 minutes, filtered, concentrated under reduced pressure and purified by high pressure liquid chromatography (eluting with 0-70% acetonitrile/water and 0.1% trifluoroacetic acid) to provide the title compound (78 mg, 78%). 1H NMR (400 MHz, methanol-d4) δ ppm 7.62 (br s, 1H), 7.51 (br s, 1H), 7.39 (br s, 1H), 6.30-6.20 (m, 1H), 4.21 (q, 2H), 3.95-3.85 (m, 1H), 3.8-3.5 (m, 4H), 3.15-2.80 (m, 4H), 2.75-2.40 (m, 3H), 2.35-2.20 (m, 2H), 2.10-1.90 (m, 2H), 1.65-1.50 (m, 1H), 1.30 (t, 3H). MS (DCI) 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-0cb8dad6b4aa4ee4b66a8a848be703d0 |
| Source note | uspto-grants-2010_11 |