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Sodium Hydroxide → HCID 68814812、化合物

HRID 730026
ノート
印刷プレビュー

反応式

HRID 730026 の反応式
[C:1]1([C:11](=[O:13])[CH3:12])[C:10]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].S([O-])([O-])(=O)=O.[Mg+2]>C1COCC1>[C:1]1([CH:11]([OH:13])[CH3:12])[C:10]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 111828801-AcetylazuleneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 68814812HCID 68814812、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-(Azulen-1-yl)ethanone (13.0 g) prepared according to a method described in the literature (Mori et al., J. Heterocycl. Chem., Vol. 33, 1996, pp. 841-846) was dissolved in dehydrated THF (380 mL), and stirried with cooling on ice under nitrogen atmosphere. This reaction mixture was carefully added with lithium aluminum hydride (1.45 g, Wako Pure Chemical Industries), and stirried with cooling on ice for 1 hour. The reaction mixture was carefully added with 2 N aqueous sodium hydroxide with cooling on ice and stirring. The reaction mixture was added with anhydrous magnesium sulfate, and stirred, then the solid was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was used for the subsequent reaction as it was.

後処理

  1. temperaturewith cooling on ice under nitrogen atmosphere
  2. temperaturewith cooling on ice for 1 hour
  3. temperaturewith cooling on ice
  4. stirringstirred
  5. customthe solid was removed by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe residue was used for the subsequent reaction as it

出典と根拠

ORDレコード
ord-ef4dd3500e6a41859c66357fde23d801
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07582658B2

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