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1-Tetralone → 2,3,4,5-tetrahydro-1H-2-benzazepin-1-one

HRID 2088731
ノート
印刷プレビュー

反応式

HRID 2088731 の反応式
[N-:1]=[N+]=[N-].[Na+].[CH2:5]1[CH2:15][C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6]1.C(=O)([O-])[O-].[K+].[K+]>Cl>[C:13]1(=[O:14])[C:12]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[CH2:6][CH2:5][CH2:15][NH:1]1
参加物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 107241-TetraloneHCID 11430Potassium CarbonateHCID 33557Sodium Azide

生成物 1

HCID 112406552,3,4,5-tetrahydro-1H-2-benzazepin-1-one

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

With cooling with ice, 2.6 g of sodium azide was added to a concentrated hydrochloric acid (60 mL) solution of 5 mL of alpha-tetralone, and stirred at room temperature for 15 hours. The reaction liquid was poured into ice water, and neutralized with potassium carbonate. This was extracted with chloroform, and the organic layer was washed with saturated saline water and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the crude product was purified through silica gel column chromatography (chloroform/methanol) to obtain 2.3 g of the entitled compound as a yellow solid.

後処理

  1. customThe reaction liquid
  2. extractionThis was extracted with chloroform
  3. washthe organic layer was washed with saturated saline water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customthe crude product was purified through silica gel column chromatography (chloroform/methanol)

出典と根拠

ORDレコード
ord-eeb231ce04fb4f78809f9c75cbd3214b
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436004B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート