HRID646255

反应详情

EQUATION

反应方程式

HRID 646255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-(3-bromo-4-fluoro-phenylethynyl)-1-ethyl-2-methanesulfonyl-1H-pyrrole (0.35 g, 0.93 mmol) in acetone was treated with NaHCO3 (0.047 g, 0.56 mmol) and MgSO4 (0.17 g, 1.4 mmol), treated with KMnO4 (0.32 g, 2.05 mmol) and water, stirred at room temperature for 2 h and fitered. The filtercake was washed with EtOAC, dried overnight and washed with EtOAc a second time. The combined filtrates were washed with H2O and brine, dried (Na2SO4) and concentrated in vacuo to yield 0.32 gm (86% yield) of an oil. This was used as is in Step 5.

WORKUP

后处理

  1. washThe filtercake was washed with EtOAC
  2. customdried overnight
  3. washwashed with EtOAc a second time
  4. washThe combined filtrates were washed with H2O and brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo