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Diisopropylethylamine → 4-Benzyl-2-cyano-1-phenylpiperazine

HRID 2393277
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인쇄 미리보기

반응식

HRID 2393277 반응식
Cl.[CH2:2]([NH:9][CH2:10][CH2:11][NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH:19]([N:22](C(C)C)CC)(C)C.[C:28]([C:30](=C)C#N)#N>CN(C=O)C>[CH2:2]([N:9]1[CH2:30][CH2:28][N:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:11]([C:19]#[N:22])[CH2:10]1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 136705Vinylidene cyanideHCID 12366334N1-Benzyl-N2-phenylethane-1,2-diamine hydrochloride

생성물 1

HCID 149987524-Benzyl-2-cyano-1-phenylpiperazine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A solution of 3 (5.07 g, 17.0 mmol) and diisopropylethylamine (4.97 g, 38.4 mmol) in DMF (40 mL) was treated with a solution of 2-cyanoacrylonitrile (2.30 g, 26.3 mmol) in DMF (40 mL) at room temperature (14 d). The solvent was removed in vacuo and the residue dissolved in dichloromethane and washed with water, brine, and dried (Na2SO4). Concentrated in vacuo, the residue was recrystallized from ethanol to afford 4 as white crystals.

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in dichloromethane
  3. washwashed with water, brine
  4. dry with materialdried (Na2SO4)
  5. concentrationConcentrated in vacuo
  6. customthe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-39fe6dfa71414307aa35e917ffdb40d5
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05807856

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