p-Toluenesulfonic acid monohydrate → 1-Methyl-5-(1,3-dioxolan-2-yl)-imidazole

HRID 1936763ノート

反応式

HRID 1936763 の反応式
[CH3:1][N:2]1[C:6]([CH:7]=[O:8])=[CH:5][N:4]=[CH:3]1.[OH2:9].[C:10]1([CH3:20])C=CC(S(O)(=O)=O)=CC=1>C(O)CO>[CH3:1][N:2]1[C:6]([CH:7]2[O:9][CH2:10][CH2:20][O:8]2)=[CH:5][N:4]=[CH:3]1

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 5735921-methyl-1H-imidazole-5-carbaldehyde

生成物 1

HCID 226098451-Methyl-5-(1,3-dioxolan-2-yl)-imidazole

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

1-Methyl-5-formyl imidazole (0.64 g) was treated with ethylene glycol (0.3 ml), p-toluenesulphonic acid monohydrate (0.0015 g) and powdered 4A molecular seives under N2 for 18 hours at reflux. Subsequent cooling and filtration was followed by washing of the organic phase with aqueous sodium carbonate solution (2N), drying and concentration to give the title compound; δH (CDCl3) 7.43 (1H,s), 7.12 (1H,s), 5.91 (1H,s), 4.10(4H,m), 3.70(3H,s).

後処理

  1. customfor 18 hours
  2. temperatureat reflux
  3. temperatureSubsequent cooling
  4. filtrationfiltration
  5. washby washing of the organic phase with aqueous sodium carbonate solution (2N)
  6. customdrying
  7. concentrationconcentration

出典と根拠

ORDレコード
ord-6d03490ed8024c9684f012036f469dc4
出典データセット
uspto-grants-2002_05
特許番号
US06391874B1

反応ノート

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