반응 #302847

ord-902f15fce91d42039a9a2c1b5220640a

반응 방정식

O=C(CC(=O)c1cc(Br)ccc1O)c1ccc([N+](=O)[O-])cc1
compound 3
O=C(CC(=O)c1cc(Br)ccc1O)c1ccc([N+](=O)[O-])cc1
1-(5-bromo-2-hydroxyphenyl)-3-(4-nitrophenyl)propan-1,3-dione
O=S(=O)(O)O
sulfuric acid
O=c1cc(-c2ccc([N+](=O)[O-])cc2)oc2ccc(Br)cc12
compound 4
O=c1cc(-c2ccc([N+](=O)[O-])cc2)oc2ccc(Br)cc12
6-bromo-4′-nitroflavone

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 3 (2.00 g, 5.49 mmol), concentrated sulfuric acid (0.5 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′-nitroflavone (compound 4). Yield: 1.79 g (yield constant: 94.2%) MS m/z 347 (MH+).

출처

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