HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetoacetate → HCID 66747120, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 5-methyl-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 10487522 | — |
| Product | HCID 66747120 | HCID 66747120 | — |
Reaction Steps
A solution of 5-methyl-1H-benzo[d][1,3]oxazine-2,4-dione (Example 12c) (1.36 g, 7.68 mmol), ethyl 3-oxobutanoate (1.46 mL, 11.5 mmol), and NaOH (0.046 g, 1.15 mmol) in anhydrous dioxane (10 mL) were refluxed under nitrogen for 15 hrs. The solvent was then removed under vacuum, and the residue was re-dissolved in DMF (15 mL). To this solution was added POCl3 (1.41 mL, 15.4 mmol), and the reaction mixture was stirred at room temperature for 45 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09000054B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-75aeadb63a5a4c2b8239a9147ecf9a97 |
| Source note | uspto-grants-2015_04 |