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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2063963Generated: October 31, 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/2063963

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 numberUS08288386B2
Source datasetuspto-grants-2012_10
ORD IDord-0a2abd93ce724ef1911944e00612ee9e
Source noteuspto-grants-2012_10