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

HRID 1861941
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HRID 1861941 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 186219114-(2-Aminoethyl)-3-fluoroaniline수율 107.1%

시약·촉매·용매 2

HCID 1118Sulfuric Acid용매
HCID 3283
Diethyl Ether
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0a31c2f536eb4f8190c0ad652209d765
출처 데이터셋
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06534546B1

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