HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 178471853, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| Reactant | Ethyl 4-bromo-2-fluoro-3-methyl-β-oxobenzenepropanoate | HCID 54193098 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178471853 | HCID 178471853 | 84.2% |
Reaction Steps
In 14 ml of methylene chloride was dissolved 0.70 g of ethyl 4-bromo-2-fluoro-3-methyl-benzoylacetate, followed by adding thereto 0.29 g of acetic anhydride and 0.33 g of N,N-dimethylformamide dimethyl acetal, and the resulting mixture was stirred at room temperature for 2 hours and then distilled under reduced pressure to remove the solvent. The resulting residue was dissolved in 10 ml of ethanol, followed by adding thereto 0.16 g of cyclopropylamine. The resulting mixture was stirred at room temperature for 12 hours and the crystals precipitated were collected by filtration to obtain 0.72 g of colorless ethyl 2-(4-bromo-2-fluoro-3-methylbenzoyl)-3-cyclopropylaminoacrylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06025370 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-4fe3d11e778f4264b45d93e5dc78adfd |
| Source note | uspto-grants-2000_02 |