HRID2101417

反应详情

EQUATION

反应方程式

HRID 2101417 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a stirring solution of 4-(ethylsulfonyl)benzoic acid (500 mg, 2.33 mmol) in THF (5 mL) at 0° C. under argon was added 1 M borane in THF solution (3.5 mL, 3.5 mmol). The reaction mixture was stirred at 70° C. for 20 min. The reaction mixture was then cooled to room temperature, and the THF was removed under reduced pressure. The residue thus obtained was diluted with methanol (5 mL) and stirred for 5 min. Methanol was then removed under reduced pressure. This process was repeated two more times to ensure complete methanolysis of any borane complex. After residual solvent removal under vacuum, 420 mg of the title compound was obtained as a colorless gum. HPLC/MS: retention time=1.373 min, [M+H]+=201.

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled to room temperature
  2. customthe THF was removed under reduced pressure
  3. customThe residue thus obtained
  4. stirringstirred for 5 min
  5. customMethanol was then removed under reduced pressure
  6. customAfter residual solvent removal under vacuum