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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2274377Generated: October 31, 2026

Citric Acid → HCID 66731962, compound

https://huagongshe.com/reaction/2274377

Reaction equation

Participants

RoleNameHCIDCharge
ReactantCitric AcidHCID 311—
ReactantAminoisobutyric acidHCID 6119—
ReactantPotassium CarbonateHCID 11430—
Reactant2-AcetylcyclohexanoneHCID 13400—
Reactant4-Bromo-N-tert-butyl-2-fluorobenzamideHCID 22336252—
CatalystCopper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)HCID 24350—
SolventWaterHCID 962—
SolventDimethylformamideHCID 6228—
ProductHCID 66731962HCID 66731962108.9%

Reaction Conditions

Temperature100 °C

Reaction Steps

The title compound, made in accordance with General Method 3, may be used to prepare compound 3 in accordance with General Method 1. N-tert-Butyl-4-bromo-2-fluorobenzamide (850 mg, 3.1 mmol), 2-aminoisobutyric acid (450 mg, 4.36 mmol), CuI (100 mg, 0.5 mmol), TEA (0.2 mL) and K2CO3 (1.0 g, 7.2 mmol) were charged in DMF (8 mL) and water (2 mL) and stirred at RT for 5 min. 2-Acetylcyclohexanone (100 mg, 0.7 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 (50 mL, 2 times). The combined organic layer was dried over Na2SO4 and concentrated to obtain 1.0 g of 2-(4-(tert-butylcarbamoyl)-3-fluorophenylamino)-2-methylpropanoic acid.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09126962B2
Source datasetuspto-grants-2015_09
ORD IDord-d16c8f1e38ce4c4aa35e2c5c22683e2c
Source noteuspto-grants-2015_09