HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 178498257, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-(Chloromethyl)pyridine | HCID 18358 | — |
| Reactant | Benzoic acid, 2,3-diamino-4-methoxy-, methyl ester (9CI) | HCID 22663264 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178498257 | HCID 178498257 | 43.6% |
Reaction Steps
A solution of methyl 2,3-diamino-4-methoxybenzoate [0.73 g, Reference Example 8(a)] and triethylamine (0.94 g) in dry dichloromethane (20 ml), at 0° C., was treated with nicotinyl chloride (0.53 g). The reaction mixture was stirred at ambient temperature for 2 hours and then evaporated. The residue was dissolved in acetic acid (8 ml) and the solution heated at 80° C. for 2 hours. After cooling to room temperature the reaction mixture was treated with water. The insoluble material was subjected to flash chromatography on silica to give the title compound (0.46 g). NMR (CDCl3): δ 4.00(s, 3H), 4.15(s, 3H), 6.70(d, 1H), 7.40(m, 1H), 7.90(d, 1H), 8.45(m, 1H), 8.75(d, 1H), 9.30(d, 1H), 10.80(s, 1H)].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06800645B1 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-fef879f45598451791b391f42dffb212 |
| Source note | uspto-grants-2004_10 |