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Potassium Sodium Tartrate → 3-chloro-N-ethyl-4-fluoroaniline

HRID 1974616
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HRID 1974616 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][C:17]=1[F:18])[NH:11][C:12](=O)[CH3:13].[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>CCOCC.C1COCC1>[Cl:7][C:8]1[CH:9]=[C:10]([CH:15]=[CH:16][C:17]=1[F:18])[NH:11][CH2:12][CH3:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 9357Potassium Sodium TartrateHCID 589188N-(3-Chloro-4-fluorophenyl)acetamideHCID 21226445Aluminium lithium hydride

생성물 1

HCID 142024823-chloro-N-ethyl-4-fluoroaniline수율 97.5%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028
Tetrahydrofuran
용매

실험 절차

A suspension of lithium aluminium hydride (44.1 g, 1.16 mmol) in absolute ether (700 ml) is treated dropwise with a solution of 3'-chloro-4'-fluoroacetanilide (BE Patent No. 891537; 109 g, 0.576 mol) in absolute THF (350 ml). The suspension obtained is stirred for 2 hours, then cooled to 0° and treated with a Rochelle salt solution (350 ml). The crystals obtained are filtered off and washed with ether. The organic solution is dried over magnesium sulphate and the solvent is distilled off under reduced pressure. There are obtained 97.5 g (97.5%) of 3-chloro-N-ethyl-4-fluoroaniline as an amorphous material.

후처리

  1. customThe suspension obtained
  2. temperaturecooled to 0°
  3. customThe crystals obtained
  4. filtrationare filtered off
  5. washwashed with ether
  6. dry with materialThe organic solution is dried over magnesium sulphate
  7. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-d75e15cedc8e4c92835accc47f92c250
출처 데이터셋
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05283248

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