HRID1993863

反应详情

EQUATION

反应方程式

HRID 1993863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Crude 3-(4-imidazol-1-ylmethylphenyl)-5-iso-butylthiophene-2-sulfonamide (prepared according to the procedure described in Example 10(c) above) was dissolved in THF (3 mL) under N2 (g). NaOH (1.0 mL, 1M, 1.0 mmol) was added to the mixture, which was then stirred for 10 min. Butanesulfonyl chloride (45 μL, 0.35 mmol) was then added, and the mixture was stirred for 24 h at room temperature. The reaction mixture was then diluted with ethyl acetate (150 mL) and washed with water and brine. The organic phase was dried over MgSO4 and the solvent was removed in vacuo. The crude product was recrystallised from acetone to yield the title compound (31.7 mg, 0.064 mmol).

WORKUP

后处理

  1. stirringthe mixture was stirred for 24 h at room temperature
  2. washwashed with water and brine
  3. dry with materialThe organic phase was dried over MgSO4
  4. customthe solvent was removed in vacuo
  5. customThe crude product was recrystallised from acetone