Piperazine → 1,4-Piperazinediacetonitrile

HRID 1470134노트

반응식

HRID 1470134 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-6aca1c668f634f9d9a71df43b9200760
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006281B2

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