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

HRID 8052
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HRID 8052 반응식
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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a32838925aa044bb98e4a272dcdd9e10
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07087632B2

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