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Aluminium lithium hydride → HCID 22100887、化合物

HRID 1458366
ノート
印刷プレビュー

反応式

HRID 1458366 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18](=O)[C:19]([N:21]2[CH2:26][CH2:25][CH:24]([C:27]4[CH:32]=[CH:31][N:30]=[CH:29][CH:28]=4)[CH2:23][CH2:22]2)=O)=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH:5]=[C:6]([CH3:8])[CH:7]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[CH3:8][C:6]1[CH:5]=[C:4]([C:9]2[NH:10][C:11]3[C:16]([C:17]=2[CH2:18][CH2:19][N:21]2[CH2:26][CH2:25][CH:24]([C:27]4[CH:28]=[CH:29][N:30]=[CH:31][CH:32]=4)[CH2:23][CH2:22]2)=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH:3]=[C:2]([CH3:1])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 22100931HCID 22100931、化合物

生成物 1

HCID 22100887HCID 22100887、化合物収率 51.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 1-[2-(3,5-dimethylphenyl)-1H-indol-3-yl]-2-(3,4,5,6-tetrahydro-2H-[4,4']bipyridinyl-1-yl)ethane-1,2-dione (148 mg in dry tetrahydrofuran) was added dropwise 2.71 mL of a 1M solution of lithium aluminum hydride in tetrahydrofuran and the mixture heated to reflux on an oil bath. After 1.5 hours the mixture was cooled and quenched by the sequential addition of 30 mL water and 4 mL ammonium hydroxide and 25 mL ethyl acetate. The mixture was filtered to remove the solids. The organic portion was washed with brine, dried over magnesium sulfate and concentrated in vacuo to give the title compound (71 mg). m/e=410 (M+H).

後処理

  1. temperaturethe mixture heated
  2. temperatureto reflux on an oil bath
  3. temperatureAfter 1.5 hours the mixture was cooled
  4. customquenched by the sequential addition of 30 mL water and 4 mL ammonium hydroxide and 25 mL ethyl acetate
  5. filtrationThe mixture was filtered
  6. customto remove the solids
  7. washThe organic portion was washed with brine
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7f79c1b1f3db40bb9b0e099f974f3134
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05849764

反応ノート

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