تفاعل #160999

معادلة التفاعل

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride

1-aminocyclohexanecarboxylic acid phenylmethyl ester

1-hydroxybenzotriazole

4-biphenylcarboxylic acid

→

title compound

المردود 85.0%

1-[(4-Biphenylcarbonyl)amino]cyclohexanecarboxylic acid phenylmethyl ester

المردود 85.0%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooling
2. 2
   تركيزthe reaction solution was concentrated under reduced pressure, ethyl acetate
3. 3
   workup.ADDITIONwas added
4. 4
   غسيلthe mixture was successively washed with water
5. 5
   تجفيفby drying with anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONAfter the solvent was distilled off under reduced pressure
7. 7
   أخرىthe residue was purified by silica gel chromatography

الإجراء التجريبي

2.11 g (11 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added to a solution of 2.33 g (10 mmol) of 1-aminocyclohexanecarboxylic acid phenylmethyl ester, 1.68 g (11 mmol) of 1-hydroxybenzotriazole and 3.23 g (10 mmol) of 4-biphenylcarboxylic acid in 120 ml of methylene chloride under ice-cooling. After the mixture was stirred at room temperature overnight, the reaction solution was concentrated under reduced pressure, 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 3.51 g (85%) of the title compound.

المصدر