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 refluxed under heating 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 refluxed
2. temperatureunder heating 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レコード

ord-699de14b46d5438cabdf744afc78e3eb

出典データセット

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08957205B2