HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67186015, compound → HCID 67188167, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67186015 | HCID 67186015 | — |
| Catalyst | Adams' catalyst | HCID 345198 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Ethanol ethylacetate | HCID 21584252 | — |
| Product | HCID 67188167 | HCID 67188167 | 65.3% |
Reaction Steps
A suspension of PtO2 (250 mg) in EtOAc (5 mL) was added to a solution of ethyl[(3,5-dichlorobenzyl) (4-nitrobenzyl)amino](oxo)acetate (2.00 g, 4.86 mmol) in EtOH/EtOAc (2/1, 90 mL) under H2 (1 atm). The reaction mixture was stirred vigorously at rt for 30 min. The reaction mixture was filtered over a pad of Celite and silica gel to remove the catalyst. The solvents were removed under reduced pressure. The residue was purified by flash chromatography over silica gel (c-Hex/EtOAc 2/1) to give the title compound as a pale yellow oil (1.21 g, 61%). 1H NMR (CDCl3, 300 MHz) δ 7.31-7.05 (m, 5H), 6.71 (m, 2H), 4.39 (m, 4H), 4.25 (br s, 2H), 1.36 (m, 3H). HPLC (Condition A), Rt: 3.4 min (HPLC purity: 94.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07592477B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-a4772267802348d3ad55d8213ec3cf84 |
| Source note | uspto-grants-2009_09 |