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Triethylamine → 6-Benzylamino-2-methylimidazo[1,2-a]pyridine-3-acetonitrile

HRID 544468
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HRID 544468 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:4][N:3]=1.C(N(CC)CC)C.Cl[CH:24]([C:28](=O)[CH3:29])[CH2:25][C:26]#[N:27]>C(#N)C>[CH2:9]([NH:8][C:5]1[CH:6]=[CH:7][C:2]2[N:3]([C:24]([CH2:25][C:26]#[N:27])=[C:28]([CH3:29])[N:1]=2)[CH:4]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 139002363-Chloro-4-oxopentanenitrileHCID 204590262-Amino-5-benzylamino pyridine

생성물 1

HCID 204590346-Benzylamino-2-methylimidazo[1,2-a]pyridine-3-acetonitrile

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 2-amino-5-benzylamino pyridine (4.0 g), triethylamine (2.1 g),3-chloro-4-oxopentanenitrile (2.7 g) and acetonitrile (50 ml) is stirred and heated under reflux for 18 hr. The solvent is removed in vacuo, and the residue is dissolved in chloroform (200 ml). The solution is washed with water (4×100 ml), dried over anhydrous potassium carbonate and the chloroform is removed in vacuo. The residue is chromatographed on silica gel (200 g) using chloroform as the eluant. The product is obtainedand crystallized from acetonitrile.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 18 hr
  3. customThe solvent is removed in vacuo
  4. dissolutionthe residue is dissolved in chloroform (200 ml)
  5. washThe solution is washed with water (4×100 ml)
  6. dry with materialdried over anhydrous potassium carbonate
  7. customthe chloroform is removed in vacuo
  8. customThe residue is chromatographed on silica gel (200 g)
  9. customThe product is obtainedand crystallized from acetonitrile

출처 및 근거

ORD 기록
ord-1acab7348d6b4a308be0540ea08a4a21
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04450164

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