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Iodine → 5-iodo-1-(3-(trifluoromethyl)phenyl)pyrimidin-2,4(1H,3H)-dione

HRID 576750
ノート
印刷プレビュー

反応式

HRID 576750 の反応式
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:4]=[C:5]([N:9]2[CH:14]=[CH:13][C:12](=[O:15])[NH:11][C:10]2=[O:16])[CH:6]=[CH:7][CH:8]=1.[I:19]I.[N+]([O-])([O-])=O.[NH4+].[Ce]>C(#N)C>[I:19][C:13]1[C:12](=[O:15])[NH:11][C:10](=[O:16])[N:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:17])[F:18])[CH:4]=2)[CH:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 807IodineHCID 57418452Ammonium cerium-nitrateHCID 86723841HCID 86723841、化合物

生成物 1

HCID 901973315-iodo-1-(3-(trifluoromethyl)phenyl)pyrimidin-2,4(1H,3H)-dione収率 160.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

To a suspension of 1-(3-(trifluoromethyl)phenyl)pyrimidin-2,4(1H,3H)-dione (prepared in Reference Example 113) (5.09 g) in acetonitrile (75 ml) were added iodine (3.03 g) and cerium ammonium nitrate (6.54 g) and the resulting mixture was stirred at 80° C. for thirty minutes. The resulting mixture was cooled to 0° C. and thereto were then added ethyl acetate (150 ml), saturated saline (50 ml) and 5% sodium hydrogen sulfite solution (100 ml) so as to separate the layer. Furthermore, the aqueous layer was extracted with ethyl acetate, and the organic layer was washed with 5% aqueous sodium hydrogen sulfite solution and saturated saline. The resulting mixture was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. To the residue were added ethyl acetate (50 ml) and hexane (100 ml) and the resulting mixture was stirred for fifteen minutes, and the precipitated solids were then collected by filtration and washed with hexane to afford 5-iodo-1-(3-(trifluoromethyl)phenyl)pyrimidin-2,4(1H,3H)-dione (7.34 g).

後処理

  1. temperatureThe resulting mixture was cooled to 0° C.
  2. customadded ethyl acetate (150 ml), saturated saline (50 ml) and 5% sodium hydrogen sulfite solution (100 ml) so as to separate the layer
  3. extractionFurthermore, the aqueous layer was extracted with ethyl acetate
  4. washthe organic layer was washed with 5% aqueous sodium hydrogen sulfite solution and saturated saline
  5. dry with materialThe resulting mixture was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionTo the residue were added ethyl acetate (50 ml) and hexane (100 ml)
  8. stirringthe resulting mixture was stirred for fifteen minutes
  9. filtrationthe precipitated solids were then collected by filtration
  10. washwashed with hexane

出典と根拠

ORDレコード
ord-8afe8595f15e41f890046e2cae0f83a5
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040516B2

反応ノート

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