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Cesium fluoride → N-[6-(furan-3-yl)-1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-indazol-3-yl]butanamide

HRID 497605
ノート
印刷プレビュー

反応式

HRID 497605 の反応式
[O:1]1[CH:5]=[CH:4][C:3](B(O)O)=[CH:2]1.[F-].[Cs+].Cl[C:12]1[CH:20]=[C:19]2[C:15]([C:16]([NH:29][C:30](=[O:34])[CH2:31][CH2:32][CH3:33])=[N:17][N:18]2[CH2:21][O:22][CH2:23][CH2:24][Si:25]([CH3:28])([CH3:27])[CH3:26])=[CH:14][CH:13]=1>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[O:1]1[CH:5]=[CH:4][C:3]([C:12]2[CH:20]=[C:19]3[C:15]([C:16]([NH:29][C:30](=[O:34])[CH2:31][CH2:32][CH3:33])=[N:17][N:18]3[CH2:21][O:22][CH2:23][CH2:24][Si:25]([CH3:28])([CH3:26])[CH3:27])=[CH:14][CH:13]=2)=[CH:2]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

6

反応物 3

HCID 25953Cesium fluoride2 回HCID 2734358Furan-3-boronic acid2 回HCID 10406687N-[6-chloro-1-[[2-(trimethylsilyl)ethoxy)methyl]-1H-indazol-3-yl)butanamide

生成物 1

HCID 10386231N-[6-(furan-3-yl)-1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-indazol-3-yl]butanamide収率 12%

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
2 回
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

457 mg of furan-3-boronic acid, 1.24 g of caesium fluoride, 13 mg of palladium acetate and finally 31 mg of 2-dicyclohexylphosphine-2-(N,N-dimethylamino)biphenyl are added to 1 g of N-[6-chloro-1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-indazol-3-yl]butanamide, described previously in Example 25, in 30 cm3 of dioxane. The mixture is then heated at about 100° C. for 23 hours. A further 457 mg of furan-3-boronic acid, 1.24 g of caesium fluoride, 13 mg of palladium acetate and finally 31 mg of 2-dicyclohexylphosphine-2-(N,N-dimethylamino)biphenyl are added and refluxing is continued for 7 hours. The mixture is then allowed to return to about 19° C. over 16 hours and then filtered through a sinter funnel and evaporated under reduced pressure (2 kPa; 50° C.). The residue is rinsed with 50 cm3 of tetrahydrofuran and 50 cm3 of distilled water. The resulting residue is taken up in 75 cm3 of ethyl acetate and 50 cm3 of distilled water. The organic phase is dried over magnesium sulphate, filtered through a sinter funnel and then evaporated under reduced pressure under the conditions described previously. The residue is purified by chromatography under an argon pressure of 50 kPa, on a column of silica gel (particle size 40-60 μm; diameter 3.5 cm), eluting with a cyclohexane/ethyl acetate mixture (80/20 by volume) and collecting 35 cm3 fractions. The fractions containing the expected product are combined and evaporated under reduced pressure (2 kPa; 50° C.). 130 mg of N-[6-(furan-3-yl)-1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-indazol-3-yl]butanamide are thus obtained in the form of an orange-coloured oil.

後処理

  1. temperaturerefluxing
  2. waitto return to about 19° C. over 16 hours
  3. filtrationfiltered through a sinter funnel
  4. customevaporated under reduced pressure (2 kPa; 50° C.)
  5. washThe residue is rinsed with 50 cm3 of tetrahydrofuran and 50 cm3 of distilled water
  6. dry with materialThe organic phase is dried over magnesium sulphate
  7. filtrationfiltered through a sinter funnel
  8. customevaporated under reduced pressure under the conditions
  9. customThe residue is purified by chromatography under an argon pressure of 50 kPa
  10. washon a column of silica gel (particle size 40-60 μm; diameter 3.5 cm), eluting with a cyclohexane/ethyl acetate mixture (80/20 by volume)
  11. customcollecting 35 cm3 fractions
  12. additionThe fractions containing the expected product
  13. customevaporated under reduced pressure (2 kPa; 50° C.)

出典と根拠

ORDレコード
ord-e81eb3cd85ea48a7849b977fa440cbf6
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06949579B2

反応ノート

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