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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2095953Generated: October 31, 2026

Diisopropylethylamine → HCID 58158644, compound

https://huagongshe.com/reaction/2095953

Reaction equation

Participants

RoleNameHCIDCharge
ReactantDiisopropylethylamineHCID 81531—
ReactantTriphosgeneHCID 94429—
ReactantSodium BicarbonateHCID 516892—
ReactantHCID 58158560HCID 58158560—
ReactantN-[6-(4-amino-2-fluorophenoxy)imidazo[1,2-a]pyridin-2-yl]cyclopropanecarboxamideHCID 58158605—
SolventTetrahydrofuranHCID 8028—
SolventTetrahydrofuran ethyl acetateHCID 21939870—
ProductHCID 58158644HCID 581586449.1%

Reaction Conditions

Temperature70 °C

Reaction Steps

To a solution of 1-(4-fluorophenyl)-6-methyltetrahydropyrimidin-2(1H)-one (240 mg, 1.1 mmol) in tetrahydrofuran (5 mL) was added bis(trichloromethyl) carbonate (170 mg, 0.57 mmol), and the mixture was stirred at 70° C. for 3.5 hr. The mixture was cooled to room temperature, a solution of N-[6-(4-amino-2-fluorophenoxy)imidazo[1,2-a]pyridin-2-yl]cyclopropanecarboxamide (250 mg, 0.76 mmol) in tetrahydrofuran (8 mL) and N,N-diisopropylethylamine (300 mg, 2.3 mmol) were added to the mixture, and the mixture was stirred at room temperature for 1 hr. Ethyl acetate/tetrahydrofuran and saturated aqueous sodium hydrogen carbonate solution were added to the mixture, and the aqueous layer was extracted 3 times with ethyl acetate/tetrahydrofuran. The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (NH silica gel, ethyl acetate/hexane=50/50→100/0) to give the title compound (29 mg, 7%) as a white solid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08445509B2
Source datasetuspto-grants-2013_05
ORD IDord-57d05293b0e44880977547021f577af8
Source noteuspto-grants-2013_05