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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 660106Generated: October 31, 2026

Toluene → HCID 66657313, compound

https://huagongshe.com/reaction/660106

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTolueneHCID 1140—
ReactantCesium carbonateHCID 10796—
Reactant3-BromobenzonitrileHCID 23381—
Reactanttert-butyl (3S)-3-aminopyrrolidine-1-carboxylateHCID 854071—
Catalystpalladium(II) acetateHCID 167845—
CatalystBinap, (A+-)-HCID 634876—
SolventWaterHCID 962—
SolventDichloromethaneHCID 6344—
ProductHCID 66657313HCID 6665731354.3%

Reaction Steps

To a toluene solution (7 ml) containing 2.82 g of 3(S)-aminopyrrolidine-1-carboxylic acid tert-butyl ester (15 mmol) and 1.82 g of 3-bromobenzonitrile (10 mmol) were added 68.5 mg of BINAP (0.11 mmol), 22.5 mg of palladium acetate (0.1 mmol) and 3.91 g of cesium carbonate (12 mmol). The mixture was heated under reflux under a nitrogen atmosphere for 8 hours. After cooling to room temperature, water was added to the reaction solution, and extraction with dichloromethane was performed. After drying over sodium sulfate and concentration under reduced pressure, the residue was then purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1). The purified product was concentrated to dryness under reduced pressure to thereby obtain 1.56 g of light yellow powdery 3(S)-(3-cyanophenylamino)pyrrolidine-1-carboxylic acid tert-butyl ester.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08084442B2
Source datasetuspto-grants-2011_12
ORD IDord-a201e920945c40818541e4e908fa9b43
Source noteuspto-grants-2011_12