반응 #302858

ord-ec8093e8f99844c7b25b43ef7239b80d

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

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 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%)

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08192717B2uspto-grants-2012_06