HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formic Acid → HCID 58902031, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Reactant | (3-Chloropyrazin-2-yl)methanamine dihydrochloride | HCID 42609650 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58902031 | HCID 58902031 | — |
Reaction Steps
To a solution of C-(3-chloro-pyrazin-2-yl)-methylamine bis-hydrochloride (6.0 g, 0.027 mol) in DMF (50 mL) was added N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (7.9 g, 0.041 mol), diisopropyl ethylamine (24.2 mL, 0.139 mol), hydrate (400.0 mg, 0.003 mol) and formic acid (1.57 mL, 0.041 mol). The reaction was left to stir at rt for 16 h under an atmosphere of nitrogen. The solvent was then removed under reduced pressure and the residue was purified by chromatography (5% DCM in hexane. 1H NMR (400 MHz, CD3OD) δ ppm 4.72 (s, 2H), 8.26 (s, 1H), 8.39 (d, J=1.77 Hz, 1H), 8.57 (d, J=2.53 Hz, 1H). MS (ES+): m/z 172.11, 174.09 [MH+]; HPLC: tR=1.57 min (OpenLynx, polar—7 min).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481733B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-3db31aa0225b469daec2bf2cb902f567 |
| Source note | uspto-grants-2013_07 |