HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosgene → HCID 5279166, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | 2-Methoxyaniline | HCID 7000 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 5279119 | HCID 5279119 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 5279166 | HCID 5279166 | 68.7% |
Reaction Steps
A solution of 2-methoxy-aniline (37 mg) in dry dichloromethane (3 ml) was treated with triethylamine (0.04 ml) followed by 20% phosgene in toluene (0.08 ml). The mixture was stirred at room temperature for 1 h, and then Intermediate 3 (37 mg) was then added, and the stirring continued for 18 h. The mixture was partitioned between water and ethyl acetate. The organic layer was passed through a hydrophobic frit and evaporated and the residue was purified on a silica gel SPE cartridge. Gradient elution with 0-5% methanol in dichloromethane gave the title compound as a colourless solid (24 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07582624B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-07f0e536cb1b4e39b954fd77df0a7e7c |
| Source note | uspto-grants-2009_09 |