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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2264573Generated: October 31, 2026

Ethyl Acetate → HCID 59596367, compound

https://huagongshe.com/reaction/2264573

Reaction equation

Participants

RoleNameHCIDCharge
ReactantEthyl AcetateHCID 8857—
ReactantSodium HydroxideHCID 14798—
Reactant2-Amino-4,6-dichloropyrimidineHCID 65522—
ReactantHCID 86618286HCID 86618286—
SolventAcetoneHCID 180—
SolventWaterHCID 962—
SolventDimethylformamideHCID 6228—
ProductHCID 59596367HCID 59596367—

Reaction Conditions

Temperature60 °C

Reaction Steps

A mixture of 567 mg (1.62 mMol) of 7-hydroxy-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid (3-trifluoromethyl-phenyl)-amide (Step 6.2), 532 mg (3.24 mMol) 2-amino-4,6-dichloro-pyrimidine and 145 mg (3.62 mMol) NaOH in 5 ml acetone, 7 ml H2O and 3 ml DMF is stirred at 60° C. for 24 h. Then it is poured into water and EtOAc, the aqueous phase separated off and extracted twice with EtOAc. The organic layers are washed with water and brine, dried (Na2SO4) and concentrated. Column chromatography (SiO2; hexane/EtOAc 2:1→3:2) gives the title compound: m.p.: 175° C.; MS: [M+1]+=478/480; Anal.: C,H,N,Cl.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07855215B2
Source datasetuspto-grants-2010_12
ORD IDord-4f08f0e704d144c2ab06f7ebdb90fbc2
Source noteuspto-grants-2010_12