Back
HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1173627Generated: November 3, 2026

Cesium carbonate → 4-[(2S,3S)-3-(tert-butyldimethylsilyloxy)-2-ethyl-5-oxopyrrolidin-1-yl]-2-(trifluoromethyl)benzonitrile

https://huagongshe.com/reaction/1173627

Reaction equation

Participants

RoleNameHCIDCharge
ReactantCesium carbonateHCID 10796—
Reactant1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 636044—
Reactant4-Iodo-2-(trifluoromethyl)benzonitrileHCID 16218337—
Reactant(4S,5S)-4-(tert-butyldimethylsilyloxy)-5-ethylpyrrolidin-2-oneHCID 67105254—
CatalystBis(dibenzylideneacetone)palladiumHCID 9811564—
SolventWaterHCID 962—
SolventTolueneHCID 1140—
SolventEthyl AcetateHCID 8857—
Product4-[(2S,3S)-3-(tert-butyldimethylsilyloxy)-2-ethyl-5-oxopyrrolidin-1-yl]-2-(trifluoromethyl)benzonitrileHCID 5955701376.3%

Reaction Conditions

Temperature80 °C

Reaction Steps

A suspension of (4S,5S)-4-(tert-butyldimethylsilyloxy)-5-ethylpyrrolidin-2-one (6.00 g), 4-iodo-2-trifluoromethylbenzonitrile (8.42 g), cesium carbonate (12.05 g), tris(dibenzylideneacetone)dipalladium(0) (1.13 g) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (2.14 g) in toluene (70 mL) was stirred at 80° C. for 18 hr. Water and ethyl acetate were added to the reaction mixture and insuluble material was filtered off. The filtrate was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=50/1→1/2) to give the title compound as a pale-yellow solid (yield: 7.76 g, 76%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07834051B2
Source datasetuspto-grants-2010_11
ORD IDord-657634dd6de1478695bf2cac7595ab3b
Source noteuspto-grants-2010_11