تفاعل #935978

معادلة التفاعل

2-chloro-5-(2-oxo-pyrrolidin-1-yl)aniline

1-(2,6-dichloro-4-tetradecyloxycarbonylphenyl)-3-ethoxy-2-pyrazolin-5-one

methanesulfonic acid

→

desired compound

1-(2,6-dichloro-4-tetradecyloxycarbonylphenyl)-3-[2-chloro-5-(2-oxo-pyrrolidin-1-yl)anilino]-2-pyrazolin-5-one

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   غسيلwashed three times with water
3. 3
   workup.DISTILLATIONAfter distilling off the solvent
4. 4
   أخرىthe residue was separated by a silica gel chromatography (
5. 5
   workup.ADDITIONa solvent mixture of ethyl acetate and chloroform as a spreading agent)

الإجراء التجريبي

A mixture of 4.4 g of 2-chloro-5-(2-oxo-pyrrolidin-1-yl)aniline, 10.2 g of 1-(2,6-dichloro-4-tetradecyloxycarbonylphenyl)-3-ethoxy-2-pyrazolin-5-one and 0.5 g of methanesulfonic acid was stirred with heating at 150° C. under reduced pressure for 12 hours. After cooling, the reaction mixture was dissolved in ethyl acetate and washed three times with water. After distilling off the solvent, the residue was separated by a silica gel chromatography (using a solvent mixture of ethyl acetate and chloroform as a spreading agent) to obtain the desired compound. By recrystallization from acetonitrile 9 g of crystals having a melting point of 143° to 146° C. were obtained.

المصدر