Reacción #61528

Ecuación de reacción

2-Bromo-N-(5-chloro-pyridin-2-yl)-acetamide

1H-Pyrazole-3,5-dicarboxylic acid diethyl ester

NaH

→

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

Disolventes

DMF

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGthe mixture stirred for 2 h at RT
2. 2
   ConcentraciónAfter concentration in vacuo the residue
3. 3
   Otrowas purified by chromatography on silica gel
4. 4
   workup.ADDITIONThe fractions containing the product
5. 5
   Otrowere evaporated

Procedimiento

To a solution of 10 g 1H-Pyrazole-3,5-dicarboxylic acid diethyl ester in 200 ml absolute DMF 1.885 g of a 60% suspension of NaH in mineral oil were added in an argon atmosphere. The mixture was stirred for 15 min at RT. 11.76 g 2-Bromo-N-(5-chloro-pyridin-2-yl)-acetamide were added and the mixture stirred for 2 h at RT. After concentration in vacuo the residue was purified by chromatography on silica gel using CH2Cl2/ethylacetate=8/2. The fractions containing the product were evaporated. Yield: 16.05 g.

Fuente