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

HRID 2306688ノート

反応式

HRID 2306688 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-4e68f1eaddfe4f6487d97a98803e857d
出典データセット
uspto-grants-2004_12
特許番号
US06828320B2

反応ノート

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