反応 #1542

ord-2d447b7bc2ec4665ad48ac9de0170d06

反応方程式

O=c1cc(C(F)(F)F)nc(-c2ccccc2)[nH]1
2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone
O=C1CCC(=O)N1Br
N-bromosuccinimide
O=c1[nH]c(-c2ccccc2)nc(C(F)(F)F)c1Br
5-bromo-2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone
収率 83.5%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITthe mixture was left
  2. 2
    workup.ADDITIONThe reaction was poured onto ice water and vacuum
  3. 3
    ろ過filtered
  4. 4
    洗浄washing well with water
  5. 5
    その他The crude product was recrystallized from ethyl acetate

実験手順

To a solution of 1.0 g (3.94 mmol) of 2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone and 20 mL of glacial acetic add was added 1.0 g (5.6 mmol) N-bromosuccinimide and the mixture was left to stir at room temperature for 16 h. The reaction was poured onto ice water and vacuum filtered, washing well with water. The crude product was recrystallized from ethyl acetate to yield 1.05 g (83.5%) of 5-bromo-2-phenyl-6-trifluoromethyl-4(3H)-pyrimidinone, as a white solid. 1H-NMR (d6DMSO) δ 7.6(3H,m); 8.15(2H,m).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726124uspto-grants-1998_03