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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1509437Generated: October 31, 2026

1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → tert-butyl (3S,5R)-3-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl}(2-methylpropyl)amino)-5-(pyrrolidin-1-ylcarbonyl)piperidine-1-carboxylate

https://huagongshe.com/reaction/1509437

Reaction equation

Participants

RoleNameHCIDCharge
Reactant1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 15908—
ReactantPyrrolidineHCID 31268—
Reactant1-HydroxybenzotriazoleHCID 75771—
ReactantSodium BicarbonateHCID 516892—
Reactant(3R,5S)-(tert-butoxycarbonyl)-5-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl}(2-methylpropyl)amino]piperidine-3-carboxylic acidHCID 58355779—
SolventDimethylformamideHCID 6228—
Producttert-butyl (3S,5R)-3-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl}(2-methylpropyl)amino)-5-(pyrrolidin-1-ylcarbonyl)piperidine-1-carboxylateHCID 5835541595.4%

Reaction Conditions

Temperature50 °C

Reaction Steps

(3R,5S)-1-(tert-Butoxycarbonyl)-5-[{[1-(4-methoxybutyl)-1H-benzimidazol-2-yl]carbonyl}(2-methylpropyl)amino]piperidine-3-carboxylic acid (400 mg) and pyrrolidine (59 mg) were dissolved in DMF (10 ml), WSC.HCL (217 mg) and HOBt (150 mg) were added, and the mixture was stirred at 50° C. for 12 hr. The reaction mixture was poured into 10% aqueous sodium bicarbonate, and the mixture was extracted with ethyl acetate. The extracts were combined and washed with brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (1:1-1:0) was concentrated under reduced pressure to give the object product (420 mg).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09221836B2
Source datasetuspto-grants-2015_12
ORD IDord-8d19b40bb6844ab5b38907743923e365
Source noteuspto-grants-2015_12