HRID505863

反应详情

EQUATION

反应方程式

HRID 505863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To an ice-cooled solution of 9-butylacridine (27.0 g, 0.115 mol) and TMEDA (4.1 mL, 0.027 mol) in THF (135 mL), was added 2.5 M n-butyllithium in hexanes (140 mL, 0.350 mol) dropwise. The mixture was stirred at 0° C. overnight and quenched with water. After stirring for an additional 0.5 hours, the reaction mixture was poured into crushed ice and extracted with ethyl acetate. The organic solution was washed with water and dried over MgSO4. The solvent was evaporated and the resulting residue was chromatographed on silica gel (hexanes:ethyl acetate=10:1 as eluent) to give 14.5 g (43%) of yellow powder.

WORKUP

后处理

  1. customquenched with water
  2. stirringAfter stirring for an additional 0.5 hours
  3. additionthe reaction mixture was poured
  4. custominto crushed ice
  5. extractionextracted with ethyl acetate
  6. washThe organic solution was washed with water
  7. dry with materialdried over MgSO4
  8. customThe solvent was evaporated
  9. customthe resulting residue was chromatographed on silica gel (hexanes:ethyl acetate=10:1 as eluent)