تفاعل #492373

معادلة التفاعل

NaOH

THF

ethyl 3-(5-(3-chloro-2-(((2′,4′-dichloro-[1,1′-biphenyl]-4-yl)amino)methyl)-5-(trifluoromethyl)phenyl)picolinamido)propanoate

HCl

→

title compound

3-(5-(3-chloro-2-(((2′,4′-dichloro-[1,1′-biphenyl]-4-yl)amino)methyl)-5-(trifluoromethyl)phenyl)picolinamido)propanoic acid

المذيبات

EtOAc

NaCl

MeOH

ظروف التفاعل

المعالجة

1. 1
   أخرىthe layers were separated
2. 2
   استخلاصThe aqueous layer was extracted with EtOAc
3. 3
   غسيلthe combined organics were washed with 4M NaCl
4. 4
   تجفيفdried (Na2SO4)
5. 5
   تركيزconcentrated
6. 6
   أخرىpurified via HPLC

الإجراء التجريبي

A 3M aqueous solution of NaOH (3.1 mL, 9.3 mmol) was added to a THF (12.6 mL) and MeOH (6.3 mL) solution of ethyl 3-(5-(3-chloro-2-(((2′,4′-dichloro-[1,1′-biphenyl]-4-yl)amino)methyl)-5-(trifluoromethyl)phenyl)picolinamido)propanoate (4.1 g, 6.3 mmol) and the resulting homogeneous mixture was heated to 40° C. After 30 min the resulting mixture was acidified with 6M aqueous HCl (1.6 mL, 9.6 mmol) diluted with EtOAc and 4M aqueous NaCl, and the layers were separated. The aqueous layer was extracted with EtOAc and the combined organics were washed with 4M NaCl, dried (Na2SO4), concentrated, and purified via HPLC to yield the title compound.

المصدر