HRID1417824

反应详情

EQUATION

反应方程式

HRID 1417824 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of (-)-(isochroman-1-yl)acetone (LXXXIV, 0.73 g), ammonium acetate (1.48 g), methanol (2.5 ml), and THF (2.5 ml) is stirred for 25 min and then acetic acid (1.5 ml) and sodium cyanoborohydride (0.48 g) are added. After stirring for 2 hr, the mixture is concentrated and the residue is stirred with dichloromethane and sodium hydroxide (4N). The mixture is extracted with dichloromethane and washed with saline/sodium hydroxide (1N). The organic phase is separated and dried over sodium sulfate to give 2-[(-)-isochroman-1-yl]-(±)-1-methylethylamine.

WORKUP

后处理

  1. stirringAfter stirring for 2 hr
  2. concentrationthe mixture is concentrated
  3. stirringthe residue is stirred with dichloromethane and sodium hydroxide (4N)
  4. extractionThe mixture is extracted with dichloromethane
  5. washwashed with saline/sodium hydroxide (1N)
  6. customThe organic phase is separated
  7. dry with materialdried over sodium sulfate