HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 11245159, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| Reactant | HCID 23141413 | HCID 23141413 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 11245159 | HCID 11245159 | 96% |
Reaction Steps
N-(4-Trifluoromethoxyphenyl)-4-methoxyisophthalamic acid (48 mg) obtained in step F, 11 mg of ammonium chloride, 25 mg of benzotriazol-1-ol monohydrate, and 31 mg of (3-dimethylaminopropyl)ethylcarbodiimide hydrochloride were dissolved in 2 mL of N,N-dimethylformamide, and 70 μL of N,N-diisopropylethylamine was added. This solution was stirred overnight at room temperature, and then the solvent was distilled off under reduced pressure. The resulting residue was purified by column chromatography (5 g of silica gel, 2 g of aminopropyl-modified silica gel) using a 100:1 mixture of dichloromethane and methanol as an elution solvent, thereby obtaining 45 mg (96%) of 3-N-(4-trifluoromethoxyphenyl)-4-methoxyisophthalamide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063046B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-72fc2f7e976f42999ce6670c9c0793cb |
| Source note | uspto-grants-2011_11 |