تفاعل #161010

معادلة التفاعل

1-aminocyclohexanecarboxylic acid phenylmethyl ester

di-t-butyl dicarbonate

triethylamine

1-(benzoyl)piperazine

→

title compound

المردود 86.1%

1-[[(4-Benzoyl-1-piperazinyl)carbonyl]amino]cyclohexanecarboxylic acid phenylmethyl ester

المردود 86.1%

المذيبات

methylene chloride

methylene chloride

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature overnight
2. 2
   تركيزAfter the reaction solution was concentrated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
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
   غسيلthe obtained crystal was washed with diethyl ether

الإجراء التجريبي

A solution of 114 mg (0.9 mmol) of N,N-dimethylaminopyridine and 2.17 g (9.3 mmol) of 1-aminocyclohexanecarboxylic acid phenylmethyl ester in methylene chloride was added to a solution of 2.03 g (9.3 mmol) of di-t-butyl dicarbonate in 60 ml of methylene chloride, and the mixture was stirred at room temperature for 30 minutes. Thereafter, a solution of 1.88 g (18.6 mmol) of triethylamine and 1.86 g (9.8 mmol) of 1-(benzoyl)piperazine in methylene chloride was added thereto, and the mixture was stirred at room temperature overnight. After the reaction solution was concentrated, the residue was dissolved in ethyl acetate, 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 obtained crystal was washed with diethyl ether to obtain 3.60 g (86%) of the title compound.

المصدر