Methyl iodide → 1-[[(3-Methyl-2-oxo-1-imidazolidinyl)carbonyl]amino]cyclohexanecarboxylic acid phenylmethyl ester

1.83 g (12.9 mmol) of methyl iodide was added to a solution of 1.50 g (4.3 mmol) of 1-[[(2-oxo-1-imidazolidinyl)carbonyl]amino]cyclohexanecarboxylic acid phenylmethyl ester and 1.78 g (12.9 mmol) of potassium carbonate in 100 ml of acetonitrile, and the mixture was heated under reflux overnight. The reaction solution was concentrated, ethyl acetate was added thereto, and the mixture was successively washed with water, a 10% aqueous potassium hydrogensulfate solution, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, followed by drying with anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the residue was purified by silica gel chromatography to obtain 710 mg (50%) of the title compound.

1. temperaturethe mixture was heated
2. temperatureunder reflux overnight
3. concentrationThe reaction solution was concentrated
4. additionethyl acetate was added
5. washthe mixture was successively washed with water
6. dry with materialby drying with anhydrous sodium sulfate
7. distillationAfter the solvent was distilled off under reduced pressure
8. customthe residue was purified by silica gel chromatography

ORD 기록

ord-96e73cfa94b34cb8b96fc1d98db4f6aa

출처 데이터셋

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08829209B2