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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 570615Generated: October 31, 2026

Citric Acid → HCID 66732558, compound

https://huagongshe.com/reaction/570615

Reaction equation

Participants

RoleNameHCIDCharge
ReactantCitric AcidHCID 311—
ReactantAminoisobutyric acidHCID 6119—
ReactantPotassium CarbonateHCID 11430—
Reactant2-AcetylcyclohexanoneHCID 13400—
Reactant4-Bromo-2-fluoro-N-propylbenzamideHCID 24697054—
CatalystCopper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)HCID 24350—
SolventWaterHCID 962—
SolventDimethylformamideHCID 6228—
ProductHCID 66732558HCID 66732558148.2%

Reaction Conditions

Temperature100 °C

Reaction Steps

The title compound, made in accordance with General Method 3, may be used to prepare compound 5 in accordance with General Method 1. 4-Bromo-2-fluoro-N-propylbenzamide (620 mg, 2.39 mmol), 2-aminoisobutyric acid (422 mg, 4.09 mmol), CuI (100 mg, 0.6 mmol), TEA (catalytic amount) and K2CO3 (1.13 g, 8.1 mmol) were dissolved in DMF (8 mL) and water (2 mL) stirred at RT for 5 min. 2-Acetylcyclohexanone (0.13 g, 0.3 mmol) was added and the reaction mixture was heated at 100° C. for 18 h. The reaction mixture was acidified with 1 M citric acid (pH 4) and extracted with ethyl acetate (100 mL, 2 times). The combined organic layer was dried over Na2SO4 and concentrated to obtain 1.0 g of 2-(4-(propylcarbamoyl)-3-fluorophenylamino)-2-methylpropanoic acid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09023869B2
Source datasetuspto-grants-2015_05
ORD IDord-766f4f1440564be48f8a312e91a51258
Source noteuspto-grants-2015_05