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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1291311Generated: October 31, 2026

Acetic Acid → HCID 69961372, compound

https://huagongshe.com/reaction/1291311

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAcetic AcidHCID 176—
ReactantHCID 18919222HCID 18919222—
CatalystNickelHCID 935—
SolventEthanolHCID 702—
Solvent1,2-DimethoxyethaneHCID 8071—
ProductHCID 69961372HCID 6996137274.8%

Reaction Conditions

Temperature40 °C

Reaction Steps

In a mixture of DME (50 ml) and ethanol (2 ml) was dissolved 3-ethyl-7-[4-(4-fluorobenzoyl)benzyl]-5-methyl-2-methylthio-7H-pyrrolo[2,3-d]pyrimidin-4(3H)-one (344 mg) followed by addition of acetic acid (224 mg), and the mixture was warmed to 40° C. Then, Raney nickel was added until disappearance of the starting compound had been verified by TLC. The catalyst was then filtered off and the solvent was distilled off under reduced pressure. The residue was dissolved in ethyl acetate, washed with saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution in that order, and dried over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure and the residue was allowed to stand, whereupon crystals separated out. This crystal crop was harvested by filtration, rinsed with ethanol and hexane, and dried to provide the title compound (230 mg).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS05753664
Source datasetuspto-grants-1998_05
ORD IDord-8a2c882e02ca49bd96fd9dd682d50f00
Source noteuspto-grants-1998_05