HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 60703790, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | 4-Bromo-3-methylaniline | HCID 23359 | — |
| Reactant | 1,4-Dioxane-2,6-dione | HCID 78232 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 60703790 | HCID 60703790 | 75.5% |
Reaction Steps
[1,4]Dioxane-2,6-dione (312 mg, 2.69 mmol) was added to a solution of 4-bromo-3-methyl-phenylamine (500 mg, 2.69 mmol) in tBuOMe (7.0 ml), and the mixture was stirred at room temperature overnight. The reaction solution was concentrated under reduced pressure. Acetic anhydride (4.0 ml, 42.3 mmol) and sodium acetate (35 mg, 0.427 mmol) were added to the resulting residue, and the mixture was heated with stirring at 60° C. for three hours. Water was added to the reaction solution, and collection by filtration and trituration with water gave 4-(4-bromo-3-methyl-phenyl)-morpholine-3,5-dione (577 mg, 73%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169254B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-2e292c38aca2476fb121fe75b397e03b |
| Source note | uspto-grants-2015_10 |