HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 22285550, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 22285397 | HCID 22285397 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22285550 | HCID 22285550 | 24% |
Reaction Steps
1-(4-Aminophenyl)-2-(2-chlorophenyl)-5-methyl-N-(1-piperidinyl)-1H-imidazole-4-carboxamide (Example 45) (51 mg, 0.12 mmol) was dissolved in dry dichloromethane (2 mL) and treated with acetic anhydride (14 μL, 0.15 mmol) dropwise. The solution was stirred at rt for 4 h, and then the solvent was evaporated to give an amber oil. It was purified by HPLC (YMC-packed Pro C18 15×200 mm column, 30-90% CH3CN in H2O/TFA, 20 mL/min.) to afford an off-white solid (13 mg, 15%): LC-MS m/z 452.3 (MH+), retention time 2.31 min (method 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06960601B2 |
| Source dataset | uspto-grants-2005_11 |
| ORD ID | ord-191de32909104df8960acccbac24a508 |
| Source note | uspto-grants-2005_11 |