反応 #159639

反応方程式

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

→

title compound ( D98 )

収率 108.0%

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

収率 108.0%

溶媒

methanol

NaOH

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度under reflux overnight
3. 3
   濃縮the mixture was concentrated in vacuo
4. 4
   workup.ADDITIONThe residue was diluted with water (10 ml)
5. 5
   抽出the resulting mixture was extracted with ethyl acetate (2×10 ml)
6. 6
   洗浄The organic solution was washed with brine (20 ml)
7. 7
   乾燥dried over Na2SO4
8. 8
   その他evaporated in vacuo

実験手順

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.

出典