1-(2-Hydroxyethyl)piperazine → HCID 22272590、化合物

HRID 1064817ノート

反応式

HRID 1064817 の反応式
[OH:1][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:17][C:18]#[N:19]>C(#N)C>[C:18]([CH2:17][N:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH2:2][OH:1])[CH2:5][CH2:6]1)#[N:19]

参加物

5

反応物 3

HCID 76771-(2-Hydroxyethyl)piperazineHCID 7856ChloroacetonitrileHCID 11430Potassium Carbonate

生成物 1

HCID 22272590HCID 22272590、化合物収率 95%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 1-(2-hydroxyethyl)piperazine (2.60 g, 20 mmol) in acetonitrile (35 ml) was added potassium carbonate (3.04 g, 22 mmol) and chloroacetonitrile (1.51 g, 20 mmol) was dropped thereinto with ice cooling. The mixture was stirred at room temperature for 30 minutes and then stirred at 45° C. for 30 minutes. This reaction mixture was filtered off, the filtrate was concentrated in vacuo and the residue was purified by a silica gel column chromatography (100 g of silica gel; developing solvent, chloroform:ammonia-saturated methanol=20:1→10:1) to provide 3.20 g (yield 95%) of 4-(cyanomethyl)piperazine-1-ethanol.

後処理

  1. additionwas dropped
  2. stirringstirred at 45° C. for 30 minutes
  3. filtrationThis reaction mixture was filtered off
  4. concentrationthe filtrate was concentrated in vacuo
  5. customthe residue was purified by a silica gel column chromatography (100 g of silica gel; developing solvent, chloroform:ammonia-saturated methanol=20:1→10:1)

出典と根拠

ORDレコード
ord-936ecfab76e64f38a98714768ecd7c58
出典データセット
uspto-grants-2005_11
特許番号
US06969711B2

反応ノート

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