Piperazine → 1,4-Piperazinediacetonitrile

HRID 45696노트

반응식

HRID 45696 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-973ea195ef5e41ec8af4edaad7a99865
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541448B2

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