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1-[3-(Trifluoromethyl)phenyl]but-1-en-3-one → HCID 61748346、化合物

HRID 2044157
ノート
印刷プレビュー

反応式

HRID 2044157 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[F:7][C:8]([F:21])([F:20])[C:9]1[CH:10]=[C:11]([CH:15]=[CH:16][C:17](=[O:19])[CH3:18])[CH:12]=[CH:13][CH:14]=1>C1COCC1>[F:7][C:8]([F:20])([F:21])[C:9]1[CH:10]=[C:11]([CH2:15][CH2:16][CH:17]([OH:19])[CH3:18])[CH:12]=[CH:13][CH:14]=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 1449341-[3-(Trifluoromethyl)phenyl]but-1-en-3-oneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 61748346HCID 61748346、化合物収率 89.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

590 mg (15.4 mmol) of LiAlH4 were added in portions at 0° C. to a solution of 2.2 g (10.3 mmol) of 4-(3-(trifluoromethyl)phenyl)but-3-en-2-one in THF (20 ml), and stirring was then carried out for 1 h at RT. The mixture was then quenched at 0° C. with a sat. aq. Na2SO4 sol. and the reaction solution was filtered over kieselguhr. The filtrate was extracted with EA (3×60 ml) and the combined organic phases were washed with water, dried over Na2SO4, filtered and concentrated in vacuo. There were obtained as residue 2.0 g (9.2 mmol, 89%) of 4-(3-(trifluoromethyl)phenyl)-butan-2-ol, which was reacted further without additional purification.

後処理

  1. customThe mixture was then quenched at 0° C. with a sat. aq. Na2SO4 sol.
  2. filtrationthe reaction solution was filtered over kieselguhr
  3. extractionThe filtrate was extracted with EA (3×60 ml)
  4. washthe combined organic phases were washed with water
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-d9e48d830362413b93145fdb6ca8b46f
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586755B2

反応ノート

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