HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methoxyacetic Acid → HCID 19012215, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methoxyacetic Acid | HCID 12251 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | 4-Methylpyridine-2,3-diamine | HCID 317495 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 19012215 | HCID 19012215 | — |
Reaction Conditions
| Temperature | 165 °C |
|---|
Reaction Steps
A mixture of 2,3-diamino-4-picoline (0.1 g, 0.81 mmol) and methoxyacetic acid (0.16 ml, 2 mmol) was heated in a sealed tube at 165° C. for 24 hours. The reaction was cooled and neutralized with NH4OH. The crude material was dissolved in methanol (2 ml) and silica-gel (10 g) was added. The dried silica-gel was then loaded on a silica-gel flash-column and eluted initially with EtOAc and then with 2% methanol in EtOAc. The pure desired compound was obtained as a cream colored solid (0.067 g, 47%). 1H-NMR (CDCl3): 8.27 (d, 1H, J=5 Hz), 7.07 (d, 1H, J=5 Hz), 4.86 (s, 2H), 3.57 (s, 3H), 2.7 (s, 3H). FAB-MS: m/e 178 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05332744 |
| Source dataset | uspto-grants-1994_07 |
| ORD ID | ord-5f4fc8a4002f402cb7550e6f7efdb6d7 |
| Source note | uspto-grants-1994_07 |