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Hydrochloric Acid → 4-[4-(Propan-2-yl)piperazin-1-yl]aniline

HRID 552386
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HRID 552386 반응식
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][CH:11]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].O.O.[Sn](Cl)Cl.Cl>CO>[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:11]=[CH:12][C:13]([NH2:16])=[CH:14][CH:15]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 61436Stannous chloride dihydrateHCID 98347891-Isopropyl-4-(4-nitrophenyl)piperazine

생성물 1

HCID 91615454-[4-(Propan-2-yl)piperazin-1-yl]aniline수율 88%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 1-isopropyl-4-(4-nitro-phenyl)-piperazine (8.3 g, 33.2 mmol) in MeOH (120 mL) is added tin (II) dichloride dihydrate (37.4 g, 0.165 mol). The mixture is cooled using a water bath and conc. HCl is added (36 mL). The reaction is stirred at room temperature overnight. After removing the methanol, the resultant solution is basified using conc. NaOH (pH 11). The water phase is extracted with diethyl ether. The combined organic layer are dried (MgSO4), filtered and the solvent is removed under reduced pressure to afford the title compound (6.4 g, 88%).

후처리

  1. temperatureThe mixture is cooled
  2. customAfter removing the methanol
  3. extractionThe water phase is extracted with diethyl ether
  4. dry with materialThe combined organic layer are dried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-c1bf0d0faa8c4af49ac84635fdf70868
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07951818B2

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