HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 51349080, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Urea | HCID 1176 | — |
| Reactant | 3-Ethoxy-4-hydroxy-5-nitrobenzaldehyde | HCID 584878 | — |
| Reactant | 1-(2-Methylphenyl)-2-phenylethan-1-one | HCID 6613313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 51349080 | HCID 51349080 | 8% |
Reaction Steps
A mixture of 2-phenyl-1-o-tolylethanone (commercially available) (200 mg, 0.95 mmol), 3-ethoxy-4-hydroxy-5-nitrobenzaldehyde (183 mg, 0.86 mmol), urea (156 mg, 2.59 mmol), concentrated HCl (0.07 mL, 0.86 mmol) in EtOH (5 mL) was refluxed overnight. Followed standard aqueous/EtOAc workup, then purified by preparative HPLC to give Compound 114 (31.75 mg, yield 8%). 1H NMR (DMSO-d6 400 MHz): δ 10.33 (br, 1H), 8.59 (s, 1H), 7.51-7.44 (m, 2H), 7.23-7.13 (m, 4H), 6.96-6.89 (m, 4H), 6.80-6.77 (m, 2H), 5.36-5.21 (m, 1H), 4.08-3.99 (m, 2H), 2.36 (s, 1.6H), 2.13 (s, 1.3H), 1.34-1.28 (m, 3H); MS (ESI): m/z 446.0 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067893B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-4c339bc1f467418bb37ed1e2fd04c923 |
| Source note | uspto-grants-2015_06 |