반응 #302854

반응 방정식

compound 14

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

sulfuric acid

→

compound 15

6-bromo-4′-methoxyflavone

용매

acetic acid

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도to reflux for 1 hour
3. 3
   기타was returned to room temperature
4. 4
   workup.ADDITIONice pieces were then added to the reaction solution
5. 5
   여과The precipitated crystal was collected by filtration

실험 절차

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).

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