反応 #1375831

ord-0715c72bda124bf98c74e734fd1917d1

反応方程式

Cn1cc(CC(=O)O)c2ccccc21
1-methyl-3-indole acetic acid
O=S(=O)(O)O
sulfuric acid
CO
methanol
COC(=O)Cc1cn(C)c2ccccc12
yellow oil
COC(=O)Cc1cn(C)c2ccccc12
methyl 2-(1-methyl-3-indolyl)acetate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The mixture was concentrated by evaporation
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in dichloromethane
  3. 3
    workup.ADDITIONpoured into a solution of aqueous saturated sodium bicarbonate
  4. 4
    抽出The mixture was then extracted with dichloromethane and excess magnesium sulfate
  5. 5
    workup.ADDITIONwas added to the extract
  6. 6
    workup.DISTILLATIONThe product was purified by distillation

実験手順

To a solution of 20 g of 1-methyl-3-indole acetic acid in 120 mL of methanol was added 0.5 mL of concentrated sulfuric acid and the mixture was stirred at room temperature for 18 hours. The mixture was concentrated by evaporation and the residue was dissolved in dichloromethane, and then poured into a solution of aqueous saturated sodium bicarbonate. The mixture was then extracted with dichloromethane and excess magnesium sulfate was added to the extract. The product was purified by distillation to give 25 g of yellow oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05747236uspto-grants-1998_05