HRID1106795

反应详情

EQUATION

反应方程式

HRID 1106795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 2-(5-bromo-2-(phenethyl)phenyl)-4,4-dimethyl-4,5-dihydrooxazole (20 g) in diethyl ether (70 ml) at 0° C. was added DIBAL (168 ml, 1 Mol solution in CH2Cl2). The mixture was stirred at ambient temperature for 18 hours and cooled to 0° C. Aqueous 2N HCl was added to destroy excess DIBAL, the resulting solid was filtered off and suspended in a mixture of water and ethyl acetate. Triethylamine was added until the white solid was dissolved. The organic layer was separated, dried (MgSO4) and evaporated to give 2-(N-(5-bromo-2-(phenethyl)benzyl)amino)-2-methylpropan-1-ol (14.21 g).

WORKUP

后处理

  1. temperaturecooled to 0° C
  2. customto destroy excess DIBAL
  3. filtrationthe resulting solid was filtered off
  4. additionsuspended in a mixture of water and ethyl acetate
  5. additionTriethylamine was added until the white solid
  6. dissolutionwas dissolved
  7. customThe organic layer was separated
  8. dry with materialdried (MgSO4)
  9. customevaporated