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Formaldehyde → [2-(3-Methylphenyl)-1H-imidazole-4,5-diyl]dimethanol

HRID 1112483
ノート
印刷プレビュー

反応式

HRID 1112483 の反応式
[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:8][CH:9]=[CH:10][N:11]=2)[CH:2]=1.[CH2:13]=[O:14].[C:15](=[O:18])([O-])[O-].[K+].[K+]>>[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[NH:11][C:10]([CH2:15][OH:18])=[C:9]([CH2:13][OH:14])[N:8]=2)[CH:2]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 712FormaldehydeHCID 11430Potassium CarbonateHCID 126227242-(3-Methylphenyl)-1H-imidazole

生成物 1

HCID 22764400[2-(3-Methylphenyl)-1H-imidazole-4,5-diyl]dimethanol収率 9%

反応条件

温度
90 °C

実験手順

A reaction vessel equipped with a stirrer and a reflux condenser was charged with 15.8 g (0.1 mole) of 2-m-tolylimidazole, 24 ml (0.3 mole) of 37% formalin and 2 g (0.015 mole) of potassium carbonate. They were heated at about 90° C. for 1 hour with stirring. The contents were cooled, and the crystals were collected by filtration. The crystals collected were boiled together with 50 ml of water, cooled, and again collected by filtration. The crystals so collected were then boiled together with 20 ml of toluene, cooled, and collected by filtration. The crystals were recrystallized from methanol to afford 2-m-tolyl-4,5-dihydroxymethyl imidazole as a final product in an amount of 2 g (yield 9%). The thin-layer chromatography (Alumina G, ethanol) of these crystals gave only one spot at Rf = 0.7.

後処理

  1. customA reaction vessel equipped with a stirrer and a reflux condenser
  2. temperatureThe contents were cooled
  3. filtrationthe crystals were collected by filtration
  4. customThe crystals collected
  5. temperaturecooled
  6. filtrationagain collected by filtration
  7. customThe crystals so collected
  8. temperaturecooled
  9. filtrationcollected by filtration
  10. customThe crystals were recrystallized from methanol

出典と根拠

ORDレコード
ord-c83c1b106c6b4ee888279b573f0cb9ec
出典データセット
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04122277

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート