Stannous Chloride → 3-Chloro-4-(4-methylpiperazin-1-yl)aniline

HRID 457572

反応式

HRID 457572 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[N:11]1[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]1.[Sn](Cl)Cl>Cl>[Cl:1][C:2]1[CH:7]=[C:6]([CH:5]=[CH:4][C:3]=1[N:11]1[CH2:12][CH2:13][N:14]([CH3:17])[CH2:15][CH2:16]1)[NH2:8]

参加物

4

反応物 2

HCID 24479Stannous ChlorideHCID 28372941-(2-Chloro-4-nitrophenyl)-4-methylpiperazine

生成物 1

HCID 8203433-Chloro-4-(4-methylpiperazin-1-yl)aniline収率 95%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To a stirred solution of 1-(2-chloro-4-nitrophenyl)-4-methylpiperazine (2.43 g, 9.5 mmol) in 2N HCl (35 mL) at RT was added tin (II) chloride (7.2 g, 38 mmol). After 1 h, the solids were collected by filtration and dissolved in aqueous 1 N NaOH (300 mL). The aqueous solution was extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine, dried over anhydrous magnesium sulfate, filtered, and evaporated to afford the title compound (2.02 g, 95%).

後処理

  1. filtrationthe solids were collected by filtration
  2. dissolutiondissolved in aqueous 1 N NaOH (300 mL)
  3. extractionThe aqueous solution was extracted with ethyl acetate (3×50 mL)
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-404738228c6c445aa5fa02486a4e59c2
出典データセット
uspto-grants-2007_03
特許番号
US07189712B2

関連ノート

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