HRID748677

反应详情

EQUATION

反应方程式

HRID 748677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-[5-(t-butyldimethylsilyloxy)-1-[4-(t-butyldimethylsilyloxy)butyl]-1-(4-chlorophenylsulfonyl)pentyl]-1,4-difluorobenzene (158 mg, 0.234 mmol) in tetrahydrofuran (4 ml) was added tetrabutylammonium fluoride (a 1M tetrahydrofuran solution, 0.702 ml, 0.702 mmol). The resulting mixture was stirred at room temperature for 24 hours. After concentration of the reaction mixture, the residue was dissolved in diethyl ether, followed by successive washing with water and brine, drying over MgSO4, and concentration. The residue thus obtained was purified by medium-pressure chromatography on a silica gel column (5% methanol-methylene chloride) to yield a colorless solid. The resulting solid was recrystallized from ethyl acetate-hexane, whereby the title compound (97.0 mg, 93%) was obtained as a colorless solid.

WORKUP

后处理

  1. washby successive washing with water and brine
  2. dry with materialdrying over MgSO4, and concentration
  3. customThe residue thus obtained
  4. customwas purified by medium-pressure chromatography on a silica gel column (5% methanol-methylene chloride)
  5. customto yield a colorless solid
  6. customThe resulting solid was recrystallized from ethyl acetate-hexane, whereby the title compound (97.0 mg, 93%)
  7. customwas obtained as a colorless solid