反応 #1583871

反応方程式

water

Quinidine

5-(methoxycarbonyl)-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic acid

Quinidine

→

(R)-5-(methoxycarbonyl)-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic acid

収率 18.6%

溶媒

methanol

反応条件

後処理

1. 1
   workup.DISSOLUTIONwas completely dissolved
2. 2
   workup.WAITThe stirring was continued for 0.5 hour
3. 3
   温度The mixture was cooled down slowly
4. 4
   その他A solid was precipitated out and
5. 5
   ろ過was filtered
6. 6
   workup.ADDITIONThe filter cake was treated with hydrochloric acid

実験手順

To a solution of 5-(methoxycarbonyl)-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic acid (700 g, 2.1 mol) in methanol (14 L) was added Quinidine (617 g, 1.90 mol). The mixture was stirred at 90° C. under reflux until Quinidine was completely dissolved. The stirring was continued for 3 hours. 4.5 L water was added. The stirring was continued for 0.5 hour. The mixture was cooled down slowly. A solid was precipitated out and was filtered. The filter cake was treated with hydrochloric acid to produce (R)-5-(methoxycarbonyl)-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic acid (130 g) in a yield of 18.6%.

出典