HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22632985, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Phosgene | HCID 6371 | — |
| Reactant | HCID 22633003 | HCID 22633003 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22632985 | HCID 22632985 | — |
Reaction Steps
Phosgene, as a 12.5% solution in toluene (9.4 mL, 12 mmol), was added to a solution of 2-amino-N-allyloxy-4,5-difluorobenzamide (Example Y-3, 2.08 g, 9.1 mmol) in 75 mL of dioxane. The solution was heated at reflux for 20 hours and then poured into 200 mL of water. The aqueous solution was extracted with ethyl acetate, and the combined organic fractions were washed with water and brine and dried over magnesium sulfate. The solution was concentrated to give 2.18 g of the title compound as a solid, mp 220-221° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06331538B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-b1d20b5a7acf4b568552aeab20ce8e06 |
| Source note | uspto-grants-2001_12 |