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Water → 4-(2-Aminoethyl)-3-fluoroaniline

HRID 1861941
ノート
印刷プレビュー

反応式

HRID 1861941 の反応式
[H-].[Li+].[Al+3].[H-].[H-].[H-].[C:7]([CH2:9][C:10]1[CH:16]=[CH:15][C:13]([NH2:14])=[CH:12][C:11]=1[F:17])#[N:8].O.[OH-].[Na+]>C(OCC)C.S(=O)(=O)(O)O>[NH2:8][CH2:7][CH2:9][C:10]1[CH:16]=[CH:15][C:13]([NH2:14])=[CH:12][C:11]=1[F:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 186219812-(4-Amino-2-fluorophenyl)acetonitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 186219114-(2-Aminoethyl)-3-fluoroaniline収率 107.1%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid溶媒
HCID 3283
Diethyl Ether
溶媒
2 回

実験手順

To a suspension of aluminum lithium hydride (76 mg) in diethyl ether (5 ml), conc. sulfuric acid (0.053 ml) was added under ice cooling and stirred at room temperature for 1 h. Subsequently, a solution of the compound (100 mg) obtained in Example 251 in diethyl ether (15 ml) was added dropwise at room temperature and heated under reflux for 18 h. To the reaction mixture, water (1 ml) and 2 N aqueous sodium hydroxide solution (10 ml) were added under ice cooling and the mixture was extracted with diethyl ether; the organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure to give 110 mg of the titled compound quantitatively.

後処理

  1. additionwas added under ice cooling
  2. temperatureheated
  3. temperatureunder reflux for 18 h
  4. extractionthe mixture was extracted with diethyl ether
  5. dry with materialthe organic layer was dried with anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0a31c2f536eb4f8190c0ad652209d765
出典データセット
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06534546B1

反応ノート

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