Reacción #61529

Ecuación de reacción

1-[(5-Chloro-pyridin-2-ylcarbamoyl)-methyl]-1H-pyrazole-3,5-dicarboxylic acid diethyl ester

HCl

→

1-[(5-Chloro-pyridin-2-ylcarbamoyl)-methyl]-1H-pyrazole-3,5-dicarboxylic acid 3-ethyl ester

Disolventes

THF

H2O

NaOH

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroTHF was removed in vacuo and water
2. 2
   Otrowas removed by lyophilization
3. 3
   OtroThe residue was purified by chromatography on silica gel
4. 4
   workup.ADDITIONThe fractions containing the product
5. 5
   Otrowere evaporated
6. 6
   Otroto give a white solid

Procedimiento

To a solution of 8 g 1-[(5-Chloro-pyridin-2-ylcarbamoyl)-methyl]-1H-pyrazole-3,5-dicarboxylic acid diethyl ester in 200 ml THF and 50 ml H2O 17.2 ml IN NaOH is added. After standing for 16 h, the solution was acidified using 1 N HCl. THF was removed in vacuo and water was removed by lyophilization. The residue was purified by chromatography on silica gel using ethyl acetate followed by CH2Cl2/MeOH/HOAC/H2O=9/1/0.1/0.1. The fractions containing the product were evaporated and lyophilized to give a white solid. Yield: 4.42 g.

Fuente