Hydrazine hydrate (1:1) → N~1~-[3-(4-Methylpiperazin-1-yl)propyl]benzene-1,4-diamine

HRID 11558

반응식

HRID 11558 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][NH:11][C:12]2[CH:17]=[CH:16][C:15]([N+:18]([O-])=O)=[CH:14][CH:13]=2)[CH2:4][CH2:3]1.O.NN>C(O)C.[Ni].O>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([CH2:8][CH2:9][CH2:10][NH:11][C:12]2[CH:13]=[CH:14][C:15]([NH2:18])=[CH:16][CH:17]=2)[CH2:6][CH2:7]1

참가 물질

6

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 21975010N-[3-(4-methylpiperazin-1-yl)propyl]-4-nitro-1-aminobenzene

생성물 1

HCID 21975027N~1~-[3-(4-Methylpiperazin-1-yl)propyl]benzene-1,4-diamine

시약·촉매·용매 3

HCID 935Nickel촉매3회HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

A suspension of 0.1385 gms. of [3-(4-methyl-piperazin-1-yl)-propyl]-(4-nitro-phenyl)-amine in 3 mL of ethanol is heated to 50° C. Once dissolution is achieved 0.144 mL hydrazine monohydrate is addded to the solution. A Raney nickel slurry in water is added to the 50° C. solution dropwise, waiting after each addition for the gas evolution to cease. Sufficient quantities of Raney nickel have been added when continued addition of Raney nickel causes no further gas evolution. The reaction is then maintained at 50° C. for an additional hour, and subsequently is cooled to room temperature. The reaction mixture is filtered through a pad of celite (rinsing the pad with methanol). N-[3-(4-Methyl-piperazin-1-yl)-propyl]-benzene-1,4-diamine (0.116 gms.) is isolated upon evaporation of the filtrate, and is subsequently used without purification in the reaction of Example 302.

후처리

  1. additionA suspension of 0.1385 gms
  2. dissolutionOnce dissolution
  3. waitwaiting
  4. additionafter each addition for the gas evolution
  5. temperaturesubsequently is cooled to room temperature
  6. filtrationThe reaction mixture is filtered through a pad of celite (
  7. washrinsing the pad with methanol)

출처 및 근거

ORD 기록
ord-eb1ff254344f4230a9d813e4b5254294
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098236B2

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