反応 #1583885

ord-f689c5b0769a49d5be4fb6ea37b8f1bb

溶媒

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONwas completely dissolved
  2. 2
    workup.WAITThe stirring was continued for half an 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 half an 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

DOI: 10.6084/m9.figshare.5104873.v1特許: US09198902B2uspto-grants-2015_12