Water → HCID 178424858、化合物

HRID 325946

反応式

HRID 325946 の反応式
Cl.Cl[CH2:3][C:4]1[N:5]=[CH:6][NH:7][CH:8]=1.CN(C)C=O.O.[C:15]1([CH3:23])[CH:20]=[C:19]([CH3:21])[CH:18]=[C:17]([CH3:22])[CH:16]=1>>[CH3:23][C:15]1[CH:20]=[C:19]([CH3:21])[CH:18]=[C:17]([CH3:22])[C:16]=1[CH2:3][C:4]1[N:5]=[CH:6][NH:7][CH:8]=1

参加物

5

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 7947MesityleneHCID 178478565HCID 178478565、化合物

生成物 1

HCID 178424858HCID 178424858、化合物

実験手順

3.0 g of 4-chloromethylimidazole hydrochloride are suspended in 20 ml of mesitylene. 5 ml of dimethylformamide are added and the reaction mixture is refluxed for 12 hours, then cooled. 30 ml of water are added, the layers are separated, and the aqueous phase is washed with chloroform. The aqueous solution is then made alkaline with sodium carbonate solution and extracted with chloroform. The combined chloroform extracts are washed with water and evaporated to dryness. The residue, which is crude 4-(2',4',6'-trimethylbenzyl)imidazole, is converted to the hydrochloride by treatment with concentrated hydrochloric acid. The hydrochloride salt melts at 166°-169° C.

後処理

  1. temperaturethe reaction mixture is refluxed for 12 hours
  2. temperaturecooled
  3. customthe layers are separated
  4. washthe aqueous phase is washed with chloroform
  5. extractionextracted with chloroform
  6. washThe combined chloroform extracts are washed with water
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-16847070d393484a890e2ce81c4eaa82
出典データセット
uspto-grants-1984_04
特許番号
US04443466

関連ノート

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