HRID1873862

反应详情

EQUATION

反应方程式

HRID 1873862 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,4-dichloro-1-(1-methoxy-2-nitro-propyl)-benzene (0.35 g, 1.32 mmol), was dissolved with i-PrOH (27 ml) and treated with 1N HCl (13.2 ml, 13.2 mmol). Zinc dust (1.73 g, 26.4 mmol) was then added in small portions over 15 minutes and the solution allowed to stir for two hours at ambient temperature. The suspension was quenched by addition of saturated NaHCO3 (45 ml), stirred for 15 minutes and filtered through a small plug of Celite, washing with ethylacetate (40 ml). The organic extract was dried over anhydrous MgSO4, filtered and the solvent was removed under reduced pressure. 240 mg (77.6% of theory) of 2-(2,4-dichlorophenyl)-2-methoxy-1-methyl-ethylamine (compound Z1.14) was obtained in the form of a colourless oil as a mixture of diastereomeres.

WORKUP

后处理

  1. customThe suspension was quenched by addition of saturated NaHCO3 (45 ml)
  2. stirringstirred for 15 minutes
  3. filtrationfiltered through a small plug of Celite
  4. washwashing with ethylacetate (40 ml)
  5. extractionThe organic extract
  6. dry with materialwas dried over anhydrous MgSO4
  7. filtrationfiltered
  8. customthe solvent was removed under reduced pressure