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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2170561Generated: November 2, 2026

1,2-Dichloroethane → HCID 178522448, compound

https://huagongshe.com/reaction/2170561

Reaction equation

Participants

RoleNameHCIDCharge
Reactant1,2-DichloroethaneHCID 11—
ReactantSodium HydroxideHCID 14798—
Reactant1-HydroxybenzotriazoleHCID 75771—
ReactantMethyl 2-(2-(pyrrolidin-1-yl)ethoxy)benzoateHCID 59733402—
ReactantHCID 178508056HCID 178508056—
SolventDimethyl SulfoxideHCID 679—
SolventWaterHCID 962—
ProductHCID 178522448HCID 17852244814%

Reaction Steps

2-(2-Pyrrolidin-1-yl-ethoxy)-benzoic acid methyl ester (0.104 g, 0.42 mmol) was treated with 2 M aqueous NaOH (20 ml) and water (20 ml). The reaction mixture was stirred at room temperature for 20 hours, then reduced in vacuo and azeotroped with toluene (3×5 ml). Water (50 ml) was added and the mixture taken to pH 5 using 1M aqueous HCl. The resulting solution was reduced in vacuo and azeotroped with toluene (3×5 ml) to give a white solid, which was combined with 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (Example 2B) (0.055 g, 0.25 mmol), EDC (0.058 g, 0.3 mmol) and HOBt (0.041 g, 0.3 mmol) and stirred at room temperature in DMSO (3 ml) for 20 hours. The reaction mixture was poured into water (30 ml) and the resultant solid was collected by filtration and dried in a vacuum oven to give the title compound as a grey solid (0.015 g, 14%). (LC/MS: Rt 2.18, [MH]+ 438.06).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09051278B2
Source datasetuspto-grants-2015_06
ORD IDord-4a117dd5e8c24226b29e4bb85af3402d
Source noteuspto-grants-2015_06