HRID430066

反应详情

EQUATION

反应方程式

HRID 430066 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Aminopropanol (1.5 g, 20 mmol) was dissolved in dry DMF and treated with 3,4-dichlorobenzyl chloride (2.62 ml, 19 mmol) followed by anhydrous potassium carbonate (1.38 g, 10 mmol). The reaction mixture was stirred at room temperature overnight. The mixture was partitioned between 1M HCl and dichloromethane, the layers separated and the aqueous phase washed with dichloromethane. The aqueous phase was adjusted to pH 12 with 1M NaOH, and extracted with dichloromethane. The organic extract was dried (MgSO4) and evaporated to afford the title compound as a colourless oil (0.96 g 22%); δH (CDCl3) 1.68-1.77 (2H, m), 2.87 (2H, t, J=5.7 Hz), 3.75 (2H, s), 3.80 (2H, t, J=5.3 Hz), 7.12-7.41 (3H, m); MS (ES+) 234 (5%, MH+), 159 (100).

WORKUP

后处理

  1. customThe mixture was partitioned between 1M HCl and dichloromethane
  2. customthe layers separated
  3. washthe aqueous phase washed with dichloromethane
  4. extractionextracted with dichloromethane
  5. extractionThe organic extract
  6. dry with materialwas dried (MgSO4)
  7. customevaporated