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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1739059Generated: November 2, 2026

Phosphorus oxychloride → HCID 18696231, compound

https://huagongshe.com/reaction/1739059

Reaction equation

Participants

RoleNameHCIDCharge
ReactantPhosphorus oxychlorideHCID 24813—
ReactantHCID 18696151HCID 18696151—
SolventDiethylformamideHCID 12051—
ProductHCID 18696231HCID 18696231116.2%

Reaction Conditions

Temperature5 °C

Reaction Steps

To a solution of 3-(2-(N-t-butoxycarbonylamino)ethoxy)-4-carbamoyl-1,2-benzisoxazole (0.15 g) in diethylformamide (1.5 ml) was added phosphorus oxychloride (0.09 g) with stirring at 5° C., and the mixture was then stirred at the same temperature for 15 minutes. The reaction mixture was poured into ice water (20 ml), extracted with ethyl acetate (twice each with 20 ml) and the combined extracts were dried over anhydrous magnesium sulphate. After filtration, the solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography with cyclohexane/ethyl acetate (4/1) as an eluent, to give the title compound (0.13 g, 93%) as a colorless powder.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05965591
Source datasetuspto-grants-1999_10
ORD IDord-145eabb2957c42f08252f5002950184d
Source noteuspto-grants-1999_10