N,N-Diethyl-1,3-propanediamine → 2-(3-Diethylamino-1-propylamino)-4-(3-diethylamino-1-propoxy)nitrobenzene

HRID 8052

反応式

HRID 8052 の反応式
F[C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])[CH:5]=[CH:4][C:3]=1[N+:17]([O-:19])=[O:18].[CH2:20]([N:22]([CH2:27][CH3:28])[CH2:23][CH2:24][CH2:25][NH2:26])[CH3:21]>C1COCC1>[CH2:20]([N:22]([CH2:27][CH3:28])[CH2:23][CH2:24][CH2:25][NH:26][C:2]1[CH:7]=[C:6]([O:8][CH2:9][CH2:10][CH2:11][N:12]([CH2:15][CH3:16])[CH2:13][CH3:14])[CH:5]=[CH:4][C:3]=1[N+:17]([O-:19])=[O:18])[CH3:21]

参加物

4

反応物 2

HCID 61011N,N-Diethyl-1,3-propanediamineHCID 220147332-Fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene

生成物 1

HCID 220147292-(3-Diethylamino-1-propylamino)-4-(3-diethylamino-1-propoxy)nitrobenzene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 2-fluoro-4-(3-diethylamino-1-propoxy)nitrobenzene (2 mmol; preparation described in Example 5) in THF (5 mL) is treated with 3-diethylamino-1-propylamine (2.4 mmol at rt. After completion of the reaction, the reaction mixture is concentrated in vacuo. The residue is redissolved in EtOAc (10 mL), washed with saturated sodium bicarbonate solution, water, and brine. The organic phase is then dried over sodium sulfate and the solvent is removed in vacuo to afford the product, 2-(3-diethylamino-1-propylamino)-4-(3-diethylamino-1-propoxy)nitrobenzene (620 mg) which was used for further transformation without further purification.

後処理

  1. customAfter completion of the reaction
  2. concentrationthe reaction mixture is concentrated in vacuo
  3. dissolutionThe residue is redissolved in EtOAc (10 mL)
  4. washwashed with saturated sodium bicarbonate solution, water, and brine
  5. dry with materialThe organic phase is then dried over sodium sulfate
  6. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-a32838925aa044bb98e4a272dcdd9e10
出典データセット
uspto-grants-2006_08
特許番号
US07087632B2

関連ノート

読み込み中…