4-((5-CHLOROPYRIDIN-2-YL)AMINO)-4-OXOBUTANOIC ACID synthesis
- Product Name:4-((5-CHLOROPYRIDIN-2-YL)AMINO)-4-OXOBUTANOIC ACID
- CAS Number:339005-94-6
- Molecular formula:C9H9ClN2O3
- Molecular Weight:228.63
Yield:339005-94-6 54%
Reaction Conditions:
in tetrahydrofuran; for 2 h;Reflux;
Steps:
A
Method A: A solution of 25 mM dicarboxylic acid anhydride dissolved in 15 ml tetrahydrofuran (10 ml for phthalic anhydride) was placed in a round bottom flask equipped with a reflux condenser and 20 mM amine dissolved in 10 ml tetrahydrofuran were added. The mixture was refluxed for 2 h. The product started to crystallise at the end of the reaction. Crystallisation was completed by cooling to 4°C for several hours. The crude product was filtered with suction and recrystallised from 95% ethanol except the phthalic acid derivative, which was recrystallised from 80% acetonitrile.
References:
EP2098510,2009,A1 Location in patent:Page/Page column 5; 7
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