反应 #302854

反应方程式

compound 14

1-(5-bromo-2-hydroxyphenyl)-3-(4-methoxyphenyl)propan-1,3-dione

sulfuric acid

→

compound 15

6-bromo-4′-methoxyflavone

溶剂

acetic acid

反应条件

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 14 (2.67 g, 7.65 mmol), concentrated sulfuric acid (0.78 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′-methoxyflavone (compound 15). Yield: 2.01 g (yield constant: 79.4%) 1H NMR (300 MHz, CDCl3) δ8.35 (s, 1H), 7.87 (d, J=9.0 Hz, 2H), 7.77 (d, J=9.0 Hz, 1H), 7.45 (d, J=9.3 Hz, 1H), 7.03 (d, J=9.0 Hz, 2H), 6.75 (s, 1H), 3.90 (s, 3H).

来源