تفاعل #161013

معادلة التفاعل

methyl iodide

1-[[(2-oxo-1-imidazolidinyl)carbonyl]amino]cyclohexanecarboxylic acid phenylmethyl ester

potassium carbonate

→

title compound

المردود 50.0%

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

المردود 50.0%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةunder reflux overnight
3. 3
   تركيزThe reaction solution was concentrated
4. 4
   workup.ADDITIONethyl acetate was added
5. 5
   غسيلthe mixture was successively washed with water
6. 6
   تجفيفby drying with anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONAfter the solvent was distilled off under reduced pressure
8. 8
   أخرىthe residue was purified by silica gel chromatography

الإجراء التجريبي

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.

المصدر