Ammonium Chloride → 1-(1-Benzyl-4-methyl-piperidin-4-yl)-4-methyl-piperazine

HRID 730633ノート

反応式

HRID 730633 の反応式
C[Mg]Cl.[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]2)([C:17]#N)[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[NH4+].[Cl-]>C1COCC1>[CH2:4]([N:11]1[CH2:16][CH2:15][C:14]([N:19]2[CH2:20][CH2:21][N:22]([CH3:25])[CH2:23][CH2:24]2)([CH3:17])[CH2:13][CH2:12]1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 579896001-Benzyl-4-(4-methyl-piperazin-1-yl)-piperidin-4-carbonitrileHCID 178418332HCID 178418332、化合物

生成物 1

HCID 672729861-(1-Benzyl-4-methyl-piperidin-4-yl)-4-methyl-piperazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

10 mL methylmagnesium chloride solution (30 mmol, 3 M in THF) were added at RT to a solution of 3.0 g (10.1 mmol) 1-benzyl-4-(4-methyl-piperazin-1-yl)-piperidin-4-carbonitrile in 50 mL dry THF and the reaction mixture was stirred for 2 h. It was combined with saturated NH4Cl solution, stirred for 10 min, extracted exhaustively with diethyl ether and the combined organic phases were dried on Na2SO4. After the elimination of the desiccant and solvent the residue was purified by chromatography (Alox, activity stage II-III, gradient DCM/MeOH 100:1 to 50:1).

後処理

  1. stirringstirred for 10 min
  2. extractionextracted exhaustively with diethyl ether
  3. customthe combined organic phases were dried on Na2SO4
  4. customAfter the elimination of the desiccant and solvent the residue was purified by chromatography (Alox, activity stage II-III, gradient DCM/MeOH 100:1 to 50:1)

出典と根拠

ORDレコード
ord-69d99ebcf57a4ac9a07f32495699c289
出典データセット
uspto-grants-2009_09
特許番号
US07582625B2

反応ノート

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