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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1356810Generated: November 3, 2026

Water → HCID 18509409, compound

https://huagongshe.com/reaction/1356810

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantSodium HydroxideHCID 14798—
ReactantPhosphorus oxychlorideHCID 24813—
ReactantHCID 18509459HCID 18509459—
SolventPyridineHCID 1049—
ProductHCID 18509409HCID 1850940985.7%

Reaction Conditions

Temperature135 °C

Reaction Steps

Compound 33 (520 mg; 1.66 mmol) was dissolved in pyridine (6 ml), and phosphorus oxychloride (1.27 g; 8.3 mmol) was added thereto. The mixture was stirred for 1 hour at 130-140° C., and then cooled. The reaction mixture was poured into water, and alkalinized with sodium hydroxide pellet. The mixture was extracted with ether (120 ml), and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1), to thereby yield 420 mg of the target compound (yield: 85.7%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06586633B1
Source datasetuspto-grants-2003_07
ORD IDord-b8a87f0af27742d1bf7aa592ca0f257b
Source noteuspto-grants-2003_07