HRID330244

反应详情

EQUATION

反应方程式

HRID 330244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2.93 Grams of 2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one oxime and 0.293 g of platinum oxide were suspended in 200 ml of acetic acid, then the suspension was reduced at room temperature under 3 atmospheric hydrogen pressure for 8 hours. After the completion of hydrogenation, the catalyst was removed by filtration, and the filtrate thus obtain was concentrated to dryness under a reduced pressure. The residue thus obtained was dissolved in 100 ml of ethanol and the pH of the solution was adjusted to about pH=1 by adding an ethanol solution saturated with hydrogen chloride gas, then this solution was again concentrated to dryness under a reduced pressure. The residue thus obtained was recrystallized from ethanoldiethyl ether to obtain 0.88 g of 1-amino-2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenylpropyl)-1H-indene hydrochloride. Colorless powdery crystals. Melting point: 187.5°-189.5° C.

WORKUP

后处理

  1. customAfter the completion of hydrogenation, the catalyst was removed by filtration
  2. customthe filtrate thus obtain
  3. concentrationwas concentrated to dryness under a reduced pressure
  4. customThe residue thus obtained
  5. concentrationthis solution was again concentrated to dryness under a reduced pressure
  6. customThe residue thus obtained
  7. customwas recrystallized from ethanoldiethyl ether