Water → Ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(1-piperazinyl)nicotinoyl]acetate

In 1.5 ml of ethanol was dissolved 140 mg of anhydrous piperazine, and to the resulting solution was added 150 mg of ethyl 2-[6-chloro-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]acetate in portions, and the resulting mixture was subjected to reaction at room temperature for 30 minutes. Subsequently, the reaction mixture was added to a mixture of 5 ml of chloroform and 5 ml of water, and the organic layer was separated, washed successively with 3 ml of water and 3 ml of saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and to the crystalline material thus obtained was added 2 ml of n-hexane, after which crystals were collected by filtration to obtain 70 mg (yield 41.2%) of ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(1-piperazinyl)nicotinoyl]acetate.

1. customthe resulting mixture was subjected to reaction at room temperature for 30 minutes
2. customthe organic layer was separated
3. washwashed successively with 3 ml of water and 3 ml of saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was removed by distillation under reduced pressure
6. customto the crystalline material thus obtained
7. filtrationafter which crystals were collected by filtration

ORD record

ord-bd1c4aec26bb401c9bcdba14c828435d

Source dataset

uspto-grants-1989_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04851535