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Water → 1-(triisopropylsilyl)-1H-pyrrolo[2,3-b]pyridine-4-carbonitrile

HRID 1693698
ノート
印刷プレビュー

反応式

HRID 1693698 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[N:8]([Si:11]([CH:18]([CH3:20])[CH3:19])([CH:15]([CH3:17])[CH3:16])[CH:12]([CH3:14])[CH3:13])[CH:9]=[CH:10][C:3]=12.O.C[C:23]([N:25](C)C)=O>[C-]#N.[Zn+2].[C-]#N.[Zn].CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[CH:18]([Si:11]([CH:15]([CH3:16])[CH3:17])([CH:12]([CH3:13])[CH3:14])[N:8]1[C:4]2[N:5]=[CH:6][CH:7]=[C:2]([C:23]#[N:25])[C:3]=2[CH:10]=[CH:9]1)([CH3:19])[CH3:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 962WaterHCID 31374DimethylacetamideHCID 114382724-Chloro-1-(triisopropylsilyl)-1H-pyrrolo[2,3-b]pyridine

生成物 1

HCID 534382901-(triisopropylsilyl)-1H-pyrrolo[2,3-b]pyridine-4-carbonitrile収率 25%

試薬・触媒・溶媒 3

HCID 11186Zinc cyanide (Zn(CN)2)触媒
HCID 23994
Zinc
触媒
HCID 178418851HCID 178418851、化合物触媒

実験手順

4-Chloro-1-triisopropylsilanyl-1H-pyrrolo[2,3-b]pyridine (2.84 g, 9.2 mmol), zinc cyanide (650 mg, 5.5 mmol), and zinc dust (120 mg, 1.8 mmol) were suspended in dimethylacetamide (40 mL). The mixture was degassed thoroughly, bis(tri-t-butylphosphine)palladium (511 mg, 0.46 mmol) was added, and the mixture was stirred at 80° C. for 3d. The mixture was poured into water (80 mL) and filtered. The solids were washed with ethyl acetate and the filtrates were combined. The organic layer was separated, washed with water and brine, dried over magnesium sulfate, and concentrated. The oily residue was triturated with hexanes, the solution was decanted and the solvent was evaporated to give 1-triisopropylsilanyl-1H-pyrrolo[2,3-b]pyridine-4-carbonitrile (676 mg, 2.25 mmol, 25% yield).

後処理

  1. customThe mixture was degassed thoroughly
  2. filtrationfiltered
  3. washThe solids were washed with ethyl acetate
  4. customThe organic layer was separated
  5. washwashed with water and brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated
  8. customThe oily residue was triturated with hexanes
  9. customthe solution was decanted
  10. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-055a418d2b2243a4a0e278ec355cb396
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08158647B2

反応ノート

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