Bromine → HCID 22385760、化合物

HRID 895145ノート

反応式

HRID 895145 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[N:8]=[CH:7][N:6]2[CH:9]=[CH:10][N:11]=[C:5]2[CH:4]=1.C([O-])(=O)C.[Na+].[Br:19]Br>C(O)(=O)C>[Br:19][C:9]1[N:6]2[CH:7]=[N:8][C:3]([C:2]([F:12])([F:1])[F:13])=[CH:4][C:5]2=[N:11][CH:10]=1

参加物

5

反応物 3

HCID 24408BromineHCID 517045Sodium AcetateHCID 223857597-(Trifluoromethyl)imidazo[1,2-c]pyrimidine

生成物 1

HCID 22385760HCID 22385760、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

To a solution of 7-trifluoromethylimidazo[1,2-c]pyrimidine (1.9239 g, 10.3 mmol) in acetic acid (40 ml) was added sodium acetate (1.265 g, 15.4 mmol), then a solution of bromine (0.529 ml, 10.3 mmol) in acetic acid (7.5 ml). The solution was stirred at room temperature for 30 min, then partitioned between saturated aqueous NaHCO3 (1 l) and ethyl acetate (500 ml). The aqueous layer (pH 8) was further extracted with ethyl acetate (500 ml), and the combined organic extracts were dried (Na2SO4) and evaporated in vacuo. The residue was purified by flash chromatography (silica gel, 20% EtOAc/isohexane) to afford 0.88 g (34% over 2 steps) of the title compound as a white solid: 1H NMR (360 MHz, CDCl3) δ 7.81 (1H, s), 7.93 (1H, s), 9.09 (1H, s).

後処理

  1. custompartitioned between saturated aqueous NaHCO3 (1 l) and ethyl acetate (500 ml)
  2. extractionThe aqueous layer (pH 8) was further extracted with ethyl acetate (500 ml)
  3. dry with materialthe combined organic extracts were dried (Na2SO4)
  4. customevaporated in vacuo
  5. customThe residue was purified by flash chromatography (silica gel, 20% EtOAc/isohexane)

出典と根拠

ORDレコード
ord-e902072ff3024f16b2a2416b57211e12
出典データセット
uspto-grants-2005_07
特許番号
US06914065B2

反応ノート

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