Butanedione → 4-Isopropoxymethyl-2-(p-methoxyphenyl)-5-methylimidazole hydrochloride

HRID 839125

反応式

HRID 839125 の反応式
[ClH:1].[CH3:2][O:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([NH2:10])=[NH:9])=[CH:6][CH:5]=1.[C:13]([C:16]([CH3:18])=O)([CH3:15])=O>C(O)(C)C>[ClH:1].[CH:4]([O:3][CH2:15][C:13]1[N:9]=[C:8]([C:7]2[CH:11]=[CH:12][C:4]([O:3][CH3:2])=[CH:5][CH:6]=2)[NH:10][C:16]=1[CH3:18])([CH3:12])[CH3:5]

参加物

4

反応物 2

HCID 650ButanedioneHCID 123262194-Methoxybenzamidine Hydrochloride

生成物 1

HCID 203258814-Isopropoxymethyl-2-(p-methoxyphenyl)-5-methylimidazole hydrochloride収率 161.9%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

To a solution of 38.4 g (0.206 mole) of p-methoxy-benzamidine hydrochloride in 1 liter of refluxing isopropyl alcohol is added 25 g (0.25 mole) of biacetyl. The mixture is stirred and refluxed for 72 hours. The solvent is removed to dryness under reduced pressure and the solid residue taken up in fresh hot isopropyl alcohol. Ether is added and, on chilling, pale yellow crystals form which are collected to give about 49.5 g (81% yield) of 4-isopropoxymethyl-2-(p-methoxyphenyl)-5-methylimidazole hydrochloride as very pale yellow crystals, m.p. 149°-150° C (dec.). Recrystallization twice from isopropyl alcohol-ether with charcoaling gives the product as white crystals, m.p. 149°-150° C (dec.).

後処理

  1. temperaturerefluxed for 72 hours
  2. customThe solvent is removed to dryness under reduced pressure
  3. additionEther is added
  4. temperatureon chilling
  5. custompale yellow crystals form which are collected

出典と根拠

ORDレコード
ord-b69325bec56f42c09d77d025d7214a05
出典データセット
uspto-grants-1978_06
特許番号
US04093811

関連ノート

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