HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 18626636, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Urea | HCID 1176 | — |
| Reactant | Methanol, magnesium salt (2:1) | HCID 164537 | — |
| Reactant | HCID 53673714 | HCID 53673714 | — |
| Product | HCID 18626636 | HCID 18626636 | 5.3% |
Reaction Steps
A mixture of 2-(4-chloro-phenyl)-4-methyl-pentanoic acid ethyl ester (508 mg, 1.99 mmol) and urea (239 mg, 3.99 mmol) in a solution of magnesium methoxide in methanol (7.4 wt %, 4.28 mL, 2.99 mmol) was heated to reflux for 24 h. The reaction mixture was then concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230-400 mesh, 50/50 hexanes/ethyl acetate) afforded [2-(4-chloro-phenyl)-4-methyl-pentanoyl]-urea (28.1 mg, 5.2%) as a white solid: mp 164-165° C.; EI-HRMS m/e calcd for C13H17ClN2O2 (M+) 268.0979, found 268.0972.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06528543B1 |
| Source dataset | uspto-grants-2003_03 |
| ORD ID | ord-ef4dd061d0564334857e8718248eeabe |
| Source note | uspto-grants-2003_03 |