N,N-Diethylethylenediamine → N-[2-(diethylamino)ethyl]-4-fluorobenzamide

HRID 1381905노트

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HRID 1381905 반응식
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[CH2:11]([N:13]([CH2:17][CH3:18])[CH2:14][CH2:15][NH2:16])[CH3:12]>O1CCCC1>[CH2:11]([N:13]([CH2:17][CH3:18])[CH2:14][CH2:15][NH:16][C:6](=[O:7])[C:5]1[CH:9]=[CH:10][C:2]([F:1])=[CH:3][CH:4]=1)[CH3:12]

참가 물질

4

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온도
0 °C

실험 절차

Add 24.4 g (0.154 mol) of p-fluorobenzoyl chloride in 100 mL of tetrahydrofuran dropwise to 17.88 g (0.154 mol) of N,N-diethylethylenediamine in 150 mL of tetrahydrofuran at 0° C. Stir at 0° C. for about 2 hr then at room temperature for about 17 hr. Concentrate the resultant solution and treat the residue with 1N NaOH until about pH=10. Extract the resultant solution with methylene chloride (2×100 mL). Dry the extract with Na2SO4 amd evaporate the solvent to give the title compound.

후처리

  1. waitat room temperature for about 17 hr
  2. concentrationConcentrate the resultant solution
  3. additiontreat the residue with 1N NaOH until about pH=10
  4. extractionExtract the resultant solution with methylene chloride (2×100 mL)
  5. customDry the
  6. extractionextract with Na2SO4
  7. customamd evaporate the solvent

출처 및 근거

ORD 기록
ord-7a859c509a7f424595c72b3867095e77
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804662

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