HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 54386067, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 19896706 | HCID 19896706 | — |
| Product | HCID 54386067 | HCID 54386067 | — |
Reaction Steps
Methyl 4-oxo-4-(3,4-dihydro-3-oxo-2H-1,4-benzoxazin-7-yl)-3-methylbutyrate (10 g) was added to chloroform (100 ml) containing POCl3 (3.5 ml) and dimethylformamide (2.8 ml) at 0° C. The mixture was heated at reflux for 3 hours then stirred at room temperature overnight. The solvent was removed at reduced pressure, the residue was basified with 10% NaOH solution and extracted with ethyl acetate. The organic layer was washed with brine, dried over MgSO4, filtered and evaporated to dryness. The residue was chromatographed on silica gel and eluted with methylene chloride. The fractions containing the Product were evaporated to dryness and the residue used without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05116837 |
| Source dataset | uspto-grants-1992_05 |
| ORD ID | ord-3448d9168f834ffeb6b2af6daad82c4d |
| Source note | uspto-grants-1992_05 |