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

HRID 552386
ノート
印刷プレビュー

反応式

HRID 552386 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-c1bf0d0faa8c4af49ac84635fdf70868
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07951818B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート