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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 571467Generated: October 31, 2026

Cesium carbonate → 5-{3-(cyanomethyl)-3-[4-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]azetidin-1-yl}-N-[(1S)-1-cyclopropylethyl]pyridine-2-carboxamide

https://huagongshe.com/reaction/571467

Reaction equation

Participants

RoleNameHCIDCharge
ReactantCesium carbonateHCID 10796—
ReactantSodium BicarbonateHCID 516892—
ReactantBinap, (A+-)-HCID 634876—
Reactant5-bromo-N-[(1S)-1-cyclopropylethyl]pyridine-2-carboxamideHCID 71207911—
Reactant{3-[4-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]azetidin-3-yl}acetonitrile hydrochlorideHCID 71207967—
Catalystpalladium(II) acetateHCID 167845—
SolventTolueneHCID 1140—
Product5-{3-(cyanomethyl)-3-[4-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]azetidin-1-yl}-N-[(1S)-1-cyclopropylethyl]pyridine-2-carboxamideHCID 7120800558.6%

Reaction Conditions

Temperature120 °C

Reaction Steps

2,2′-Bis(diphenylphosphino)-1,1′-binaphthyl (91.1 mg, 0.146 mmol, Aldrich: Cat. #481084) was added to a mixture of {3-[4-(1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]azetidin-3-yl}acetonitrile hydrochloride (0.445 g, 1.00 mmol), 5-bromo-N-[(1S)-1-cyclopropylethyl]pyridine-2-carboxamide (0.273 g, 1.01 mmol), and cesium carbonate (0.971 g, 2.98 mmol) in toluene (10 mL) under N2, followed by palladium acetate (32.2 mg, 0.143 mmol). The reaction mixture was stirred at 120° C. overnight. The reaction mixture was worked up with aqueous NaHCO3, and extracted with ethyl acetate (3×30 mL). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column with ethyl acetate in hexane (0-70%) to afford the desired product (0.350 g, 58.6%). LCMS (M+H)+: m/z=597.3.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09023840B2
Source datasetuspto-grants-2015_05
ORD IDord-2234781717264293899a849229163df7
Source noteuspto-grants-2015_05