반응 #159639

반응 방정식

methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate

→

title compound ( D98 )

수율 108.0%

5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinic acid

수율 108.0%

용매

methanol

NaOH

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도under reflux overnight
3. 3
   농축the mixture was concentrated in vacuo
4. 4
   workup.ADDITIONThe residue was diluted with water (10 ml)
5. 5
   추출the resulting mixture was extracted with ethyl acetate (2×10 ml)
6. 6
   세척The organic solution was washed with brine (20 ml)
7. 7
   건조dried over Na2SO4
8. 8
   기타evaporated in vacuo

실험 절차

To an ice cooled solution of methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate (D72) (165 mg, 0.520 mmol) in methanol (10 ml), 10N NaOH (10 ml) was added. The mixture was heated under reflux overnight. After cooled to room temperature, the mixture was concentrated in vacuo. The residue was diluted with water (10 ml), acidified with 2.5N HCl (pH 1-2), and the resulting mixture was extracted with ethyl acetate (2×10 ml). The organic solution was washed with brine (20 ml), dried over Na2SO4 and evaporated in vacuo to afford the title compound (D98) (170 mg) as a red solid.

출처