Piperazine → 1,4-Piperazinediacetonitrile

HRID 870187ノート

反応式

HRID 870187 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-31b748765a7b46be858b876b33b62a78
出典データセット
uspto-grants-2015_03
特許番号
US08969377B2

反応ノート

読み込み中…