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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 552670Generated: October 31, 2026

Water → HCID 25216631, compound

https://huagongshe.com/reaction/552670

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantDimethylacetamideHCID 31374—
ReactantAzane;hydrateHCID 12896473—
ReactantHCID 86654457HCID 86654457—
CatalystZinc cyanide (Zn(CN)2)HCID 11186—
CatalystZincHCID 23994—
CatalystFerrocene-1,1'-bis-(diphenylphosphine)HCID 635956—
CatalystBis(dibenzylideneacetone)palladiumHCID 9811564—
ProductHCID 25216631HCID 25216631—

Reaction Conditions

Temperature100 °C

Reaction Steps

In a solution of 0.20 g of N-(5-bromo-2-pyrimidinyl)-4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-methyl benzoic acid amide synthesized in Step 1 of Synthetic Example 13 in 3 mL of N,N-dimethylacetamide, 0.082 g of zinc cyanide, 0.011 g of zinc, 0.013 g of tris(dibenzylideneacetone)dipalladium and 0.015 g of 1,1′-bis(diphenylphosphino)ferrocene were added, and stirred under nitrogen atmosphere at 100° C. for 2 hours. After the completion of the reaction, the reaction mixture was left and cooled to room temperature, and 20 mL of concentrated ammonia water and 20 mL of water were added, and extracted with ethyl acetate (20 mL×2). The organic phases were washed with water, and dehydrated with and dried over saturated sodium chloride aqueous solution and anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (1:1) to obtain 0.15 g of the aimed product as white crystal.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07951828B1
Source datasetuspto-grants-2011_05
ORD IDord-26885e8d15184337b1f7616f3dae0f31
Source noteuspto-grants-2011_05