HRID15241

反应详情

EQUATION

反应方程式

HRID 15241 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Methoxy-dibenzothiophene (ii)(4.3 g, 20.0 mmol) was dissolved in glacial acetic acid (60 ml) and to this solution was added fuming nitric acid (3.37 ml) in a dropwise fashion ensuring that the temperature of the mixture did not rise above 25° C. The yellow suspension was stirred for a further 45 minutes before being poured carefully into water (200 ml) and stirred for 15 minutes. The yellow solid was removed by filtration and washed thoroughly with copious amounts of water and then hexanes. The residue thus obtained was then dried in a vacuum oven to give the title compound as a yellow solid which was used without any further purification. (5.19 g, 97%) m/z (LC-MS, ESP), RT=4.15 min, (M+H)=260.1

WORKUP

后处理

  1. customdid not rise above 25° C
  2. stirringstirred for 15 minutes
  3. customThe yellow solid was removed by filtration
  4. washwashed thoroughly with copious amounts of water
  5. customThe residue thus obtained
  6. customwas then dried in a vacuum oven