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

HRID 1381905ノート

反応式

HRID 1381905 の反応式
[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]

参加物

4

反応物 2

HCID 60993N,N-DiethylethylenediamineHCID 678794-Fluorobenzoyl chloride

生成物 1

HCID 14664351N-[2-(diethylamino)ethyl]-4-fluorobenzamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7a859c509a7f424595c72b3867095e77
出典データセット
uspto-grants-1989_02
特許番号
US04804662

反応ノート

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