Piperazine → 1,4-Piperazinediacetonitrile

HRID 1479399ノート

反応式

HRID 1479399 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:14][C:15]#[N:16].[C:17](#[N:19])[CH3:18]>>[N:1]1([CH2:18][C:17]#[N:19])[CH2:6][CH2:5][N:4]([CH2:14][C:15]#[N:16])[CH2:3][CH2:2]1

参加物

5

反応物 4

HCID 4837PiperazineHCID 6342Acetonitrile2 回HCID 11430Potassium CarbonateHCID 11534Bromoacetonitrile

生成物 1

HCID 2581991,4-Piperazinediacetonitrile

実験手順

To a solution of piperazine (6 g, 69.77 mmol, 1.00 equiv) in acetonitrile (150 mL) was added potassium carbonate (19.2 g, 139.13 mmol, 2.00 equiv) and the mixture was stirred. To this was added dropwise a solution of 2-bromoacetonitrile (16.7 g, 140.34 mmol, 2.00 equiv) in acetonitrile (100 mL) and the suspension was stirred for 4 h at room temperature. The solids were filtered out and the resulting solution was concentrated under vacuum. The crude product was purified by re-crystallization from methanol resulting in 7.75 g (68%) of Intermediate 50.1 as a white solid.

後処理

  1. stirringthe suspension was stirred for 4 h at room temperature
  2. filtrationThe solids were filtered out
  3. concentrationthe resulting solution was concentrated under vacuum
  4. customThe crude product was purified by re-crystallization from methanol resulting in 7.75 g (68%) of Intermediate 50.1 as a white solid

出典と根拠

ORDレコード
ord-d7afb7006fdf4de68c57fdee5caf9652
出典データセット
uspto-grants-2016_08
特許番号
US09408840B2

反応ノート

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