Hydrochloric Acid → (S)-4-(3-methylpiperazin-1-yl)benzonitrile hydrochloride

HRID 1644991ノート

反応式

HRID 1644991 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[C@@H:11]([CH3:22])[CH2:10]2)=[CH:5][CH:4]=1)#[N:2].[ClH:23]>O1CCOCC1.C(OCC)C>[ClH:23].[CH3:22][C@@H:11]1[NH:12][CH2:13][CH2:14][N:9]([C:6]2[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[CH:4][CH:5]=2)[CH2:10]1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 58324511(S)-tert-butyl 4-(4-cyanophenyl)-2-methylpiperazine-1-carboxylate

生成物 1

HCID 66775307(S)-4-(3-methylpiperazin-1-yl)benzonitrile hydrochloride収率 94%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒

実験手順

(S)-tert-butyl 4-(4-cyanophenyl)-2-methylpiperazine-1-carboxylate (0.404 g, 1.340 mmol) was diluted with 4.0M HCl in dioxane (3 mL) and stirred for 30 min. The thick white precipitate that formed was diluted with ethyl ether (10 mL) and stirred until a fine suspension resulted. The precipitate was filtered under nitrogen and dried in vacuum to afford a white solid (300 mg, 94%). [M+H] calc'd for C12H15N3, 201; found, 201.

後処理

  1. customThe thick white precipitate that formed
  2. stirringstirred until a fine suspension
  3. customresulted
  4. filtrationThe precipitate was filtered under nitrogen
  5. customdried in vacuum

出典と根拠

ORDレコード
ord-a5120807d0de4145a20d57a8ba986135
出典データセット
uspto-grants-2012_02
特許番号
US08124606B2

反応ノート

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