HRID2101515

反应详情

EQUATION

反应方程式

HRID 2101515 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Methyl 3-chloro-5-iodobenzoate was dissolved in anhydrous THF and cooled to 0° C. 1M DIBAL in toluene (13 mL) was added slowly to the reaction solution at that temperature. The reaction mixture was stirred overnight at room temperature. Next morning, another 10 mL of 1M DIBAL in toluene was added and stirred for additional 4 h. When the reaction was complete, the reaction mixture was quenched with saturated solution of potassium sodium tartrate. The reaction mixture wad then extracted with ethyl acetate (×3). The combined organic extracts were dried over Na2SO4 and concentrated to afford the desired (3-chloro-5-iodo-phenyl)-methanol (2.7 g, 98%).

WORKUP

后处理

  1. stirringstirred for additional 4 h
  2. customthe reaction mixture was quenched with saturated solution of potassium sodium tartrate
  3. extractionThe reaction mixture wad then extracted with ethyl acetate (×3)
  4. dry with materialThe combined organic extracts were dried over Na2SO4
  5. concentrationconcentrated