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Triphenylphosphine Oxide → HCID 136200884、化合物

HRID 1619669
ノート
印刷プレビュー

反応式

HRID 1619669 の反応式
I[C:2]1[CH:7]=[C:6]([C:8]2[CH:9]=[N:10][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:12][CH:13]=2)[CH:5]=[CH:4][C:3]=1[OH:18].C([Sn](CCCC)(CCCC)[C:24]1[CH:29]=[CH:28][N:27]=[N:26][CH:25]=1)CCC.[F-].[Cs+].C1(P(=O)(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(#N)C.[Cu](I)I.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[N:26]1[CH:25]=[CH:24][C:29]([C:2]2[CH:7]=[C:6]([C:8]3[CH:9]=[N:10][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:12][CH:13]=3)[CH:5]=[CH:4][C:3]=2[OH:18])=[CH:28][N:27]=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

8

反応物 4

HCID 13097Triphenylphosphine OxideHCID 25953Cesium fluorideHCID 64097334-(Tributylstannyl)pyridazineHCID 580423402-Iodo-4-(6-(trifluoromethyl)pyridin-3-yl)phenol

生成物 1

HCID 136200884HCID 136200884、化合物

試薬・触媒・溶媒 3

HCID 83717Copper iodide
触媒
HCID 9811564Bis(dibenzylideneacetone)palladium触媒
HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

2-Iodo-4-(6-(trifluoromethyl)pyridin-3-yl)phenol (Preparation 60, 840 mg, 2.30 mmol) was dissolved in acetonitrile (20 mL) and 4-(tributylstannyl)pyridazine (1.10 g, 2.99 mmol), caesium fluoride (698 mg, 4.60 mmol), copper iodide (87 mg, 0.46 mmol) and tetrakis(triphenylphosphine)palladium (0) (266 mg, 0.23 mmol) were added. The reaction mixture was stirred at 80° C. for 18 hours and then partitioned between ethyl acetate and water containing 0.88 ammonia. The resulting mixture was stirred for 15 minutes and then filtered through a pad of celite. The aqueous phase was separated and extracted with ethyl acetate (2×20 mL) and the combined organic phases were washed with brine, dried over anhydrous MgSO4, filtered and concentrated in vacuo. The residue was purified on silica gel by Biotage (10% to 100% EtOAc in heptane over 25 CV) to give a mixture of the title compound and triphenylphosphine oxide. The residue was triturated with dichloromethane to give the title compound (360 mg, 50%) as a white solid.

後処理

  1. custompartitioned between ethyl acetate and water containing 0.88 ammonia
  2. stirringThe resulting mixture was stirred for 15 minutes
  3. filtrationfiltered through a pad of celite
  4. customThe aqueous phase was separated
  5. extractionextracted with ethyl acetate (2×20 mL)
  6. washthe combined organic phases were washed with brine
  7. dry with materialdried over anhydrous MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified on silica gel by Biotage (10% to 100% EtOAc in heptane over 25 CV)
  11. customto give

出典と根拠

ORDレコード
ord-2db79a1e469a4cc298b616b0ee2928f1
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772293B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート