Piperazine → 1,4-Piperazinediacetonitrile

HRID 1479399노트

반응식

HRID 1479399 반응식
[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

참가 물질

5

반응물 4

HCID 4837PiperazineHCID 6342Acetonitrile2회HCID 11430Potassium CarbonateHCID 11534Bromoacetonitrile

생성물 1

HCID 2581991,4-Piperazinediacetonitrile

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d7afb7006fdf4de68c57fdee5caf9652
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09408840B2

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