HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 53328240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | N,N-Dimethylglycine | HCID 673 | — |
| Reactant | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Reactant | HCID 70945143 | HCID 70945143 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 53328240 | HCID 53328240 | — |
Reaction Steps
EDCI (290 mg) was added to the mixture of 2-(dimethylamino)acetic acid (155 mg), methyl-6-(4-(3-(methylamino)propyl)-3-(trifluoromethyl)phenyl)-1H-[1,2,3]-triazolo[4,5-c]pyridine-4-carbonitrile, triethylamine (0.5 ml) in THF (5 ml). The mixture was stirred at rt for 5 hours, then diluted with ethyl acetate (100 ml), washed with sodium bicarbonate (50 ml), brine (50 ml), dried over sodium sulphate, solvent removed, residue dissolved in MeOH/NMP (3:1, 6 ml), and purified by basic hplc to give free base which was then converted to HCl salt as usual (70 mg). 1H NMR (CD3OD) δ: 8.68 (s, 1H), 8.5 (s, 1H), 8.46 (d, 1H), 7.65 (d, 1H), 4.47 (s, 3H), 4.27 (s, 2H), 3.60 (t, 2H), 3.04 (s, 3H), 2.96 (s, 6H), 2.90 (t, 2H), 1.95 (m, 2H). MS m/z 460 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115126B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-e3e44717ae49422b8bbe982b19aed6ad |
| Source note | uspto-grants-2015_08 |