HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → Formate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Chloro-p-anisic acid | HCID 169982 | — |
| Reactant | 3-aminomethyl-N-(4-dimethylaminomethyl-phenyl)-benzamide | HCID 44819544 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Formate | HCID 283 | 423.1% |
| Product | HCID 25054307 | HCID 25054307 | — |
Reaction Steps
A reaction vial was charged with 3-chloro-4-methoxybenzoic acid (40 mg, 0.21 mmol), 3-aminomethyl-N-(4-dimethylaminomethyl-phenyl)-benzamide (40 mg, 0.14 mmol), EDC (40 mg, 0.25 mmol) and HOBt (40 mg, 0.29 mmol). DMF (2 mL) was added followed by Hunig's base (0.11 mL, 0.57 mmol). The mixture was stirred at room temperature for 16 h. The product was purified by preparative HPLC using an acetonitrile/water/formic acid gradient providing the title compound as a formate salt (20 mg, 31% yield); MS, electrospray, 452 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08093266B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-332f0387552244a0a63ba1c192ea222c |
| Source note | uspto-grants-2012_01 |