反応 #302854

反応方程式

compound 14

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

sulfuric acid

→

compound 15

6-bromo-4′-methoxyflavone

溶媒

acetic acid

反応条件

後処理

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

実験手順

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).

出典