HRID5001

反应详情

EQUATION

反应方程式

HRID 5001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

An ethanol solution containing 120 g of 2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one, 45 of hydroxylamine hydrochloride and 200 ml of pyridine in 1,200 ml of ethanol was refluxed for 4 hours. After the reaction was completed, the reaction mixture was concentrated to dryness under a reduced pressure, then the residue thus obtained was dissolved in 2 liters of ethyl acetate and washed three times with 1 liter of water each time, and the residue was dried again under a reduced pressure. Recrystallized from ethyl acetate/n-hexane mixture to obtain 90 g of 2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one oxime. Light yellow flake-like crystals. Melting point: 146° C. (Decomposed).

WORKUP

后处理

  1. temperaturewas refluxed for 4 hours
  2. concentrationthe reaction mixture was concentrated to dryness under a reduced pressure
  3. customthe residue thus obtained
  4. washwashed three times with 1 liter of water each time
  5. customthe residue was dried again under a reduced pressure
  6. customRecrystallized from ethyl acetate/n-hexane mixture