HRID215794

反应详情

EQUATION

反应方程式

HRID 215794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of NaH (10 mmol, 40 mg 60%) in 4 mL of DMF was added 10 mmol of 5-fluoroisatin in 2 mL of DMF. After 15 min, a solution of 5-chloroisatoic anhydride in 3 mL of DMF was added. The reaction mixture was stirred for 18 h, methanol (0.5 mL) and 20 mL of chloroform was added and the organic solution was washed with water, dried (MgSO4) and concentrated to give a residue that was purified by silica gel chromatography (CHCl3:CH3OH). Yield 77%: mp 280-282° C.

WORKUP

后处理

  1. washthe organic solution was washed with water
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated
  4. customto give a residue that
  5. customwas purified by silica gel chromatography (CHCl3:CH3OH)