HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 22633003, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | 2-Amino-4,5-difluorobenzoic acid | HCID 735965 | — |
| Reactant | O-Allylhydroxylamine hydrochloride | HCID 3084724 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22633003 | HCID 22633003 | 53.6% |
Reaction Steps
Carbonyldiimidazole (3.37 g, 20 mmol) was added to a suspension of 4,5-difluoroanthranilic acid (3.0 g, 17 mmol) in 80 mL of THF, and the mixture was heated to reflux for 2 hours. The solution was cooled and O-allylhydroxylamine hydrochloride (1.89 g, 17 mmol) and triethylamine (2.8 mL, 20 mmol) were added, and the mixture was heated to reflux for 17 hours. The reaction mixture was concentrated and washed with 1N HCl, saturated NaHCO3, and brine and dried over magnesium sulfate. The solution was concentrated and purified by column chromatography (silica gel, CHCl3/MeOH, 98:2) to give 2.08 g of the title compound as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06331538B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-42664aa8c5f64180be6047cd23c6fb86 |
| Source note | uspto-grants-2001_12 |