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Sodium hydride → HCID 178526264、化合物

HRID 748531
ノート
印刷プレビュー

反応式

HRID 748531 の反応式
[H-].[Na+].[N:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2[CH:10]=[C:11]3[C:15](=[CH:16][CH:17]=2)[NH:14][C:13](=[O:18])[CH2:12]3)[CH:4]=1.Cl[C:20]1[CH:25]=[CH:24][C:23]([CH2:26][N:27]2[CH2:32][CH2:31][O:30][CH2:29][CH2:28]2)=[CH:22][N+:21]=1[O-:33]>CN(C)C=O>[N:27]1([CH2:26][C:23]2[CH:24]=[CH:25][C:20]([C:12]3[C:11]4[C:15](=[CH:16][CH:17]=[C:9]([C:5]5[CH:4]=[N:3][CH:8]=[CH:7][CH:6]=5)[CH:10]=4)[NH:14][C:13]=3[OH:18])=[N+:21]([O-:33])[CH:22]=2)[CH2:32][CH2:31][O:30][CH2:29][CH2:28]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 24758Sodium hydrideHCID 12050204HCID 12050204、化合物HCID 85873132HCID 85873132、化合物

生成物 1

HCID 178526264HCID 178526264、化合物収率 82.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
130 °C

実験手順

To a suspension of sodium hydride (0.05 g, 1.2 mmol, 60% dispersion in oil, pre-washed with hexane) in N,N-dimethylformamide (3 mL) was added a solution of 5-pyridin-3-yl-1,3-dihydro-2H-indol-2-one (0.19 g, 0.90 mmol) in N,N-dimethylformamide (4 mL). The mixture was stirred for 20 min under nitrogen atmosphere. 2-Chloro-5-(morpholin-4-ylmethyl)pyridine 1-oxide (0.14 g, 0.60 mmol), dissolved in N,N-dimethylformamide (3 mL) was added dropwise and the mixture was stirred at room temperature for 2 h and then heated at 130° C. for 1.5 h. The solvent was evaporated in vacuo and the residue was partitioned between 2 M HCl and ethyl acetate and the phases were separated. The aqueous layer was alkalized by addition of NaHCO3 (s) and extracted with ethyl acetate. The organic layer was dried (Na2SO4) and the solvent was removed in vacuo affording 200 mg of the title compound as a yellow solid: MS (ES) m/z 403 (M++1).

後処理

  1. additionwas added dropwise
  2. stirringthe mixture was stirred at room temperature for 2 h
  3. customThe solvent was evaporated in vacuo
  4. customthe residue was partitioned between 2 M HCl and ethyl acetate
  5. customthe phases were separated
  6. additionThe aqueous layer was alkalized by addition of NaHCO3 (s)
  7. extractionextracted with ethyl acetate
  8. dry with materialThe organic layer was dried (Na2SO4)
  9. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-bf24637a24874f8993ce87b74853f523
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399780B2

反応ノート

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