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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1693458Generated: October 31, 2026

Dimethylamine, hydrochloride → 5-Chloro-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid (1-(S)-benzyl-2-dimethylcarbamoyl-2-(S)-hydroxyethyl)amide

https://huagongshe.com/reaction/1693458

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDimethylamine, hydrochlorideHCID 10473—
Reactant1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 15908—
Reactant1-HydroxybenzotriazoleHCID 75771—
ReactantDiisopropylethylamineHCID 81531—
Reactant3-(S)-[(5-Chloro-1H-pyrrolo[2,3-c]pyridine-2-carbonyl)amino]-2-(S)-hydroxy-4-phenylbutyric acidHCID 11187952—
SolventDimethylformamideHCID 6228—
SolventSodium chloride; waterHCID 57417360—
Product5-Chloro-1H-pyrrolo[2,3-c]pyridine-2-carboxylic acid (1-(S)-benzyl-2-dimethylcarbamoyl-2-(S)-hydroxyethyl)amideHCID 59753745—

Reaction Steps

Dimethylamine hydrochloride (7 mg, 0.085 mmol) was added to a solution of 3-(S)-[(5-chloro-1H-pyrrolo[2,3-c]pyridine-2-carbonyl)amino]-2-(S)-hydroxy-4-phenylbutyric acid (EXAMPLE 124, 30 mg, 0.080 mmol), HOBt (14 mg, 0.091 mmol), DIPEA (31 μL, 0.18 mmol) and EDCI (18 mg, 0.094 mmol) in DMF (3 mL). After the addition of DIPEA (14 ml, 0.080 mmol) the mixture was stirred for 12 h before adding to diluted brine (100 mL, water/brine: 1/1). Extraction with ethyl acetate (4×25 mL), washing of the combined extracts with brine (50 mL) and drying (MgSO4) gave, after concentration, a residue which was purified by preparative LCMS to give the title compound as a colourless solid. m/z (ES+)=401.28 [M+H]+; RT=3.06 min.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08158622B2
Source datasetuspto-grants-2012_04
ORD IDord-1cc158403c6a43c4a47c1431e5d9ccb6
Source noteuspto-grants-2012_04