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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1666028Generated: October 30, 2026

1-Bromo-2,4-difluorobenzene → (2S,4S)-1-Boc-4-[(2,4-difluorophenyl)amino]-2-[(4-methylpiperazin-1-yl)carbonyl]pyrrolidine

https://huagongshe.com/reaction/1666028

Reaction equation

Participants

RoleNameHCIDCharge
Reactant1-Bromo-2,4-difluorobenzeneHCID 67674—
Reactant2-(Di-tert-butylphosphino)biphenylHCID 2734215—
ReactantSodium t-butoxideHCID 23676156—
Reactant(2S,4S)-1-Boc-4-amino-2-[(4-methylpiperazin-1-yl)carbonyl]pyrrolidineHCID 67358152—
CatalystBis(dibenzylideneacetone)palladiumHCID 9811564—
SolventTolueneHCID 1140—
Product(2S,4S)-1-Boc-4-[(2,4-difluorophenyl)amino]-2-[(4-methylpiperazin-1-yl)carbonyl]pyrrolidineHCID 6735844078%

Reaction Conditions

Temperature110 °C

Reaction Steps

(2S,4S)-1-Boc-4-amino-2-[(4-methylpiperazin-1-yl)carbonyl]pyrrolidine (10.61 g, 33.96 mmol) obtained in Step C was dissolved in toluene (100 mL). Sodium t-butoxide (3.73 g, 38.81 mmol), 2-(di-t-butylphosphino)biphenyl (863 mg, 2.89 mmol), Tris(dibenzylideneacetone)-dipalladium(0) (1.73 g, 1.93 mmol) and 1-bromo-2,4-difluorobenzene (7.48 g, 38.81 mmol) were added thereto and the reaction solution was stirred for 10 hours at 110° C. After the reaction was completed, solid like material was filtered using the Cellite from the reaction solution. The reaction solution was diluted with EtOAc and washed with water. The extracted organic solution was dried over MgSO4, concentrated in vacuo and purified by column chromatography (eluent: MC:MeOH=10/1) to give the title compound (11.24 g, 78%).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08039622B2
Source datasetuspto-grants-2011_10
ORD IDord-2942fe299a2549f1b528eb038c6c8f5f
Source noteuspto-grants-2011_10