تفاعل #69028

معادلة التفاعل

3-bromo-5-fluorobenzonitrile

piperidine-4-carboxylic acid

triethylamine

N,N-dimethylacetamide

→

1-(3-bromo-5-cyanophenyl)piperidine-4-carboxylic acid

المذيبات

EtOAc

water

ظروف التفاعل

المعالجة

1. 1
   أخرىThe organic layer was separated
2. 2
   تجفيفdried (MgSO4)
3. 3
   تركيزconcentrated
4. 4
   أخرىto give a crude reside which
5. 5
   أخرىwas purified by chromatography on silica gel (CH2Cl2/MeOH)

الإجراء التجريبي

A mixture of 3-bromo-5-fluorobenzonitrile (1.6 g, 7.8 mmol), piperidine-4-carboxylic acid (2.6 g, 12.0 mmol), triethylamine (4.0 mL, 28.5 mmol) and N,N-dimethylacetamide (1.5 mL) in a sealed tube was heated to 130° C. for 48 hr. The reaction mixture was diluted with EtOAc and water. The organic layer was separated, dried (MgSO4), and concentrated to give a crude reside which was purified by chromatography on silica gel (CH2Cl2/MeOH) to afford 1-(3-bromo-5-cyanophenyl)piperidine-4-carboxylic acid.

المصدر