HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl formate → HCID 178491157, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl formate | HCID 8025 | — |
| Reactant | HCID 178491154 | HCID 178491154 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178491157 | HCID 178491157 | — |
Reaction Steps
To a solution of 2-[(trans-4-aminocyclohexyl)amino]-N-(3,4-dimethoxybenzyl)-5nitrobenzamide (10 g) in dimethylformamide (60 mL) was added ethyl formate (200 mL), and the mixture was heated for 8 hours under reflux. The mixture was partitioned between ethyl acetate and water. The separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by a silica gel column chromatography eluting with a mixture of chloroform and methanol (20: 1). The obtained product was recrystallized from ethanol to give N-(3,4-dimethoxybenzyl)-2-[(trans-4-formamidocyclohexyl)amino]-5-nitrobenzamide as yellow crystals (7.21 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06384080B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-dfceb20c3c674344911241a0ef18b4bb |
| Source note | uspto-grants-2002_05 |