HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 86245269, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 6-Methoxy-3-pyridinylamine | HCID 81121 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86245269 | HCID 86245269 | 95.4% |
Reaction Steps
To a solution of 5-amino-2-methoxypyridine (1.00 g, 8.06 mmol) and pyridine (1.96 ml, 24.2 mmol) in tetrahydrofuran (20 ml) was added 2,2,2-trichloroethyl chloroformate (1.67 ml, 12.1 mmol) with ice-cooling, the mixture was stirred for 30 minutes with ice-cooling, the reaction mixture was poured into ice-water and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain the desired product (2.30 g, 95.4%) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07851473B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-5a4b0072bc974f17954edd84775fe5e2 |
| Source note | uspto-grants-2010_12 |