HRID66325

反应详情

EQUATION

反应方程式

HRID 66325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.1 g of 2-ethoxyphenylglyoxal (crude oil) are dissolved in 20 ml of ethanol, and 1.85 g of 3,4-dimethoxyphenethylamine are added thereto. The solution is stirred at room temperature for 30 minutes, whereby a solution containing α-(3,4-dimethoxyphenethylimino)-2-methoxyacetophenone is obtained. 0.6 g of sodium borohydride is added gradually to said solution under ice-cooling, and the mixture is stirred at room temperature for one hour. The reaction mixture is evaporated to remove solvent. Water is added to the thus obtained residue. Then, the aqueous mixture is extracted with chloroform. The extract is washed with water, dried and then evaporated to remove solvent. The oily residue thus obtained is treated with hydrochloric acid and recrystallized from a mixture of isopropanol and ether. 3.1 g of α-(3,4-dimethoxyphenethylaminomethyl)-2-ethoxybenzylalcohol hydrochloride are obtained. M.p. 169°-170° C.

WORKUP

后处理

  1. customis obtained
  2. temperaturecooling
  3. stirringthe mixture is stirred at room temperature for one hour
  4. customThe reaction mixture is evaporated
  5. customto remove solvent
  6. additionWater is added to the thus obtained residue
  7. extractionThen, the aqueous mixture is extracted with chloroform
  8. washThe extract is washed with water
  9. customdried
  10. customevaporated
  11. customto remove solvent
  12. customThe oily residue thus obtained
  13. customrecrystallized from a mixture of isopropanol and ether