HRID1936219

反应详情

EQUATION

反应方程式

HRID 1936219 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.6 g (1.32 mmol) [2-(2,2-dimethyl-4H-benzo[1,3]dioxin-6-yl)-2-hydroxyethyl]-6-[4-phenylbutoxy)hexylamine in 20 ml of a 1:1 H2O/MeOH mixture is added 0.15 ml (1.75 mmol) 35% HCl. After allowing the reaction to stir for 48 hr at room temperature, the MeOH is evaporated off at reduced pressure. The resulting aqueous mixture is extracted with 20 ml CH2Cl2. The organic phase is washed sequentially with 20 ml of a saturated NaHCO3 solution and further 20 ml H2O, dried on anhydrous Na2SO4 and evaporated to dryness to yield 0.24 g (43.9%) 2-hydroxymethyl-4-{1-hydroxy-2-[6-(4-phenylbutoxy)hexylamino]ethyl}phenol.

WORKUP

后处理

  1. customthe reaction
  2. customthe MeOH is evaporated off at reduced pressure
  3. extractionThe resulting aqueous mixture is extracted with 20 ml CH2Cl2
  4. washThe organic phase is washed sequentially with 20 ml of a saturated NaHCO3 solution and further 20 ml H2O
  5. dry with materialdried on anhydrous Na2SO4
  6. customevaporated to dryness