تفاعل #160998

معادلة التفاعل

triethylamine

1-aminocyclohexanecarboxylic acid phenylmethyl ester

phenylacetyl chloride

→

title compound

المردود 91.3%

1-[(Phenylacetyl)amino]cyclohexanecarboxylic acid phenylmethyl ester

المردود 91.3%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   درجة الحرارةunder ice-cooling
3. 3
   تركيزThe reaction solution was concentrated under reduced pressure, ethyl acetate
4. 4
   workup.ADDITIONwas 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

1.21 g (12 mmol) of triethylamine was added to a solution of 2.33 g (10 mmol) of 1-aminocyclohexanecarboxylic acid phenylmethyl ester in 100 ml of tetrahydrofuran, 1.55 g (10 mmol) of phenylacetyl chloride was added dropwise thereto under ice-cooling, and the mixture was stirred 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 3.21 g (91%) of the title compound.

المصدر