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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1963874Generated: October 31, 2026

Dichloromethane → HCID 66936842, compound

https://huagongshe.com/reaction/1963874

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDichloromethaneHCID 6344—
ReactantSodium CarbonateHCID 10340—
Reactant2-Fluoropyridine-4-boronic acidHCID 2783396—
ReactantHCID 86650609HCID 86650609—
CatalystBis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)HCID 178418228—
SolventMethanolHCID 887—
Solvent1,2-DimethoxyethaneHCID 8071—
SolventEthyl AcetateHCID 8857—
ProductHCID 66936842HCID 6693684241.7%

Reaction Conditions

Temperature105 °C

Reaction Steps

To 6-chloro-N-(3-fluorobenzyl)-4-(trifluoromethyl)pyridin-2-amine (70 mg, 0.230 mmol) was added 2-fluoropyridin-4-ylboronic acid (58.3 mg, 0.414 mmol), PdCl2(dppf).CH2Cl2 adduct (22.52 mg, 0.028 mmol), DME (1.2 ml), and 2M sodium carbonate (0.460 ml, 0.919 mmol). The resulting reaction mixture was stirred at 105° C. until completion as indicated by LCMS, about 6 hours. The reaction mixture was cooled, 15 ml of ethyl acetate and 5 ml of methanol was added, filtered and concentrated to yield a crude solid. The solid was purified by prep LC. The product was free-based using 200 ml of ethyl acetate and washed with saturated sodium bicarbonate (1×), water (2×), saturated salt solution (1×), dried sodium sulfate, filtered and concentrated to a constant mass, yielding 35 mg of titled compound as free base. LCMS (m/z): 366.2 (MH+), retention time=1.20 min.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08415381B2
Source datasetuspto-grants-2013_04
ORD IDord-71bb082d07b644e18b1747617c8c6913
Source noteuspto-grants-2013_04