反应 #302847

ord-902f15fce91d42039a9a2c1b5220640a

反应方程式

O=C(CC(=O)c1cc(Br)ccc1O)c1ccc([N+](=O)[O-])cc1
compound 3
O=C(CC(=O)c1cc(Br)ccc1O)c1ccc([N+](=O)[O-])cc1
1-(5-bromo-2-hydroxyphenyl)-3-(4-nitrophenyl)propan-1,3-dione
O=S(=O)(O)O
sulfuric acid
O=c1cc(-c2ccc([N+](=O)[O-])cc2)oc2ccc(Br)cc12
compound 4
O=c1cc(-c2ccc([N+](=O)[O-])cc2)oc2ccc(Br)cc12
6-bromo-4′-nitroflavone

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度to reflux for 1 hour
  3. 3
    其他was returned to room temperature
  4. 4
    workup.ADDITIONice pieces were then added to the reaction solution
  5. 5
    过滤The precipitated crystal was collected by filtration

实验过程

A mixed solution consisting of compound 3 (2.00 g, 5.49 mmol), concentrated sulfuric acid (0.5 ml), and acetic acid (40 ml) was heated to reflux for 1 hour. The temperature of the resultant was returned to room temperature, and ice pieces were then added to the reaction solution. The precipitated crystal was collected by filtration, so as to obtain a product of interest, 6-bromo-4′-nitroflavone (compound 4). Yield: 1.79 g (yield constant: 94.2%) MS m/z 347 (MH+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08192717B2uspto-grants-2012_06