Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1196844Generated: November 1, 2026

Chloroform → HCID 54386067, compound

https://huagongshe.com/reaction/1196844

Reaction equation

Participants

RoleNameHCIDCharge
ReactantChloroformHCID 6212—
ReactantDimethylformamideHCID 6228—
ReactantPhosphorus oxychlorideHCID 24813—
ReactantHCID 19896706HCID 19896706—
ProductHCID 54386067HCID 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

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05116837
Source datasetuspto-grants-1992_05
ORD IDord-3448d9168f834ffeb6b2af6daad82c4d
Source noteuspto-grants-1992_05