3-(4,5-dihydro-1H-imidazol-2-yl)pyridine → 3-(1H-Imidazol-2-yl)pyridine

HRID 485796

反応式

HRID 485796 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:8][CH2:9][CH2:10][N:11]=2)[CH:2]=1.[Mn]([O-])([O-])(=O)=O.[Ba+2]>C(Cl)Cl>[NH:8]1[CH:9]=[CH:10][N:11]=[C:7]1[C:3]1[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 2380793-(4,5-dihydro-1H-imidazol-2-yl)pyridineHCID 3084030Barium manganate

生成物 1

HCID 123955003-(1H-Imidazol-2-yl)pyridine収率 65.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-(3-pyridyl)imidazoline (7.2 g, 0.049M), and barium manganate (52.5 g) in CH2Cl2 (500 ml) were refluxed for 24 hrs. The reaction mixture was then filtered through diatomaceous earth, washed with ethylacetate (3×200 ml) and methanol (3×100 ml). The combined filtrates were concentrated to yield an oil which was purified on silica gel column, eluted with 20% by volume methanol 80% by volume methylene dichloride, to give 3-(1H-imidazol-2-yl)pyridine (4.66 g, 64.7%).

後処理

  1. filtrationThe reaction mixture was then filtered through diatomaceous earth
  2. washwashed with ethylacetate (3×200 ml) and methanol (3×100 ml)
  3. concentrationThe combined filtrates were concentrated
  4. customto yield an oil which
  5. customwas purified on silica gel column
  6. washeluted with 20% by volume methanol 80% by volume methylene dichloride

出典と根拠

ORDレコード
ord-10d4d0afa5b84f799de819521cbe7aa2
出典データセット
uspto-grants-1985_08
特許番号
US04537969

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