HRID1734688

反应详情

EQUATION

反应方程式

HRID 1734688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

N-trityl-1-[4-(benzoxazol-2-yl)benzyloxy]-3-hydroxy-2-propanamine (0.4 g; 0.74 mmol) is added to a suspension of potassium hydride (0.12 g; 1. mmol; 35% suspension in oil) in dry THF (4 ml) at 0° C. The reaction is stirred for 15 minutes at 20° C. 4-Phenyl-1-butyl iodide (0.21 g; 0.81 mmol) is added and the reaction mixture stirred for 15 hours. The reaction is quenched with MeOH, diluted with CH2Cl2 and washed with water 2x. The organic phase is dried (Na2SO4), concentrated and purified by column chromatography with 80% CH2Cl2 /20% petroleum ether to yield N-trityl-1-[4-(benzoxazol-2-yl)benzyloxy]-3-(4-phenylbutoxy)-2-propanamine as an oil which is used directly in Step F.

WORKUP

后处理

  1. stirringthe reaction mixture stirred for 15 hours
  2. customThe reaction is quenched with MeOH
  3. additiondiluted with CH2Cl2
  4. washwashed with water 2x
  5. dry with materialThe organic phase is dried (Na2SO4)
  6. concentrationconcentrated
  7. custompurified by column chromatography with 80% CH2Cl2 /20% petroleum ether