反应 #302858

ord-ec8093e8f99844c7b25b43ef7239b80d

反应方程式

COc1ccc(O)c(C(=O)CC(=O)c2ccc([N+](=O)[O-])cc2)c1
compound 22
COc1ccc(O)c(C(=O)CC(=O)c2ccc([N+](=O)[O-])cc2)c1
1-(5-methoxy-2-hydroxyphenyl)-3-(4-nitrophenyl)propan-1,3-dione
O=S(=O)(O)O
sulfuric acid
COc1ccc2oc(-c3ccc([N+](=O)[O-])cc3)cc(=O)c2c1
6-methoxy-4′-nitroflavone
COc1ccc2oc(-c3ccc([N+](=O)[O-])cc3)cc(=O)c2c1
compound 23

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 22 (2.92 g, 9.26 mmol), concentrated sulfuric acid (1 ml), and acetic acid (50 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-methoxy-4′-nitroflavone (compound 23). Yield: 2.31 g (yield constant: 84.1%)

来源

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