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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2276324Generated: October 31, 2026

Binap, (A+-)- → 4-(1'-Cyclopropylmethyl-2'-oxo-3,4,5,6,1',2'-hexahydro-2H-[1,4']bipyridinyl-4-yl)-benzoic acid

https://huagongshe.com/reaction/2276324

Reaction equation

Participants

RoleNameHCIDCharge
ReactantBinap, (A+-)-HCID 634876—
ReactantMethyl 4-(piperidin-4-yl)benzoateHCID 24904226—
Reactant4-Bromo-1-(cyclopropylmethyl)pyridin-2(1H)-oneHCID 58554515—
Catalystpalladium(II) acetateHCID 167845—
SolventTolueneHCID 1140—
SolventEthyl AcetateHCID 8857—
Product4-(1'-Cyclopropylmethyl-2'-oxo-3,4,5,6,1',2'-hexahydro-2H-[1,4']bipyridinyl-4-yl)-benzoic acidHCID 59497101—

Reaction Conditions

Temperature100 °C

Reaction Steps

4-Piperidin-4-ylbenzoic acid methyl ester (0.40 g, 1.81 mmol), palladium(II) acetate (0.015 g, 0.069 mmol) sodium tert-butoxide (0.34 g, 3.44 mmol) and BINAP (0.06 g, 0.096 mmol) were added to a stirred solution of intermediate D3 (0.31 g, 1.37 mmol) in toluene (10 ml). The reaction mixture was heated at 100° C. for 16 hours in a sealed tube. After cooling to room temperature the mixture was diluted with EtOAc and then filtered through diatomaceous earth, after which the solvent was evaporated in vacuo. The crude residue was treated with a mixture of DCM/methanol and then filtered off. The filtrate was evaporated to dryness in vacuo to yield crude D37 (0.48 g, 100%) that was used without further purification.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09132122B2
Source datasetuspto-grants-2015_09
ORD IDord-6aeb2cab14ec43cdadcf3a56086726e8
Source noteuspto-grants-2015_09