Formaldehyde → [2-(2-Methylphenyl)-1H-imidazole-4,5-diyl]dimethanol

HRID 1112486ノート

反応式

HRID 1112486 の反応式
[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[NH:8][CH:9]=[CH:10][N:11]=1.C=O.[C:15](=[O:18])([O-])[O-].[K+].[K+].[CH3:21][O:22]CCO>O>[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[NH:11][C:10]([CH2:15][OH:18])=[C:9]([CH2:21][OH:22])[N:8]=1

参加物

6

反応物 4

HCID 712FormaldehydeHCID 80192-MethoxyethanolHCID 11430Potassium CarbonateHCID 114692151H-Imidazole, 2-(2-methylphenyl)-

生成物 1

HCID 22764398[2-(2-Methylphenyl)-1H-imidazole-4,5-diyl]dimethanol収率 5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 15.8 g (0.1 mole) of 2-o-tolylimidazole 9 g (0.3 mole) of paraformaldehyde, 2 g (0.015 mole) of potassium carbonate and 50 ml of methyl cellosolve was heated at 90° C. for 30 minutes with stirring in the same way as in Example 1. Then, 200 ml of water was added, and the reaction mixture was boiled for a while and cooled. The crystals were collected by filtration, boiled together with 20 g of toluene, and collected by filtration. The crystals collected were dissolved in acetone, and a small amount of activated carbon was added. The mixture was filtered, and the filtrate was evaporated to dryness to afford 2-o-tolyl-4,5-dihydroxymethyl imidazole as a final product in an amount of 1 g (yield 5%). The thin-layer chromatography (alumina G, ethanol) of the crystals gave only one spot at Rf = 0.6-0.8.

後処理

  1. temperaturecooled
  2. filtrationThe crystals were collected by filtration
  3. filtrationcollected by filtration
  4. customThe crystals collected
  5. dissolutionwere dissolved in acetone
  6. additiona small amount of activated carbon was added
  7. filtrationThe mixture was filtered
  8. customthe filtrate was evaporated to dryness

出典と根拠

ORDレコード
ord-537bc3dfc1194049bd178b4a9442a70b
出典データセット
uspto-grants-1978_10
特許番号
US04122277

反応ノート

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