Potassium Carbonate → 4-((4-Methylpiperazin-1-yl)methyl)benzonitrile

HRID 357659ノート

反応式

HRID 357659 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(=O)([O-])[O-].[K+].[K+].[C:14]([C:16]1[CH:23]=[CH:22][C:19]([CH2:20]Br)=[CH:18][CH:17]=1)#[N:15]>O1CCCC1.O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:20][C:19]2[CH:22]=[CH:23][C:16]([C:14]#[N:15])=[CH:17][CH:18]=2)[CH2:4][CH2:3]1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 869964-(Bromomethyl)benzonitrile

生成物 1

HCID 75376124-((4-Methylpiperazin-1-yl)methyl)benzonitrile収率 42.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Under the argon atmosphere, 4-methylpiperazine (2.00 g, 20.0 mmole) and potassium carbonate (3.41 g, 24.7 mole) were added to a solution of 4-cyanobenzyl bromide (3.20 g, 16.3 mole) in tetrahydrofuran (30 ml). After stirring at room temperature for 18 hours, the mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water followed by a saturated aqueous saline, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give 4-(4-methyl-1-piperazinylmethyl)benzonitrile as a colorless crystalline powder (1.49 g, 42.4%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-8bccc00daeb0424ca3293b744836ca8f
出典データセット
uspto-grants-1998_11
特許番号
US05840895

反応ノート

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