Thionyl Chloride → 5-(Chloromethyl)-1-Ethyl-1H-Imidazole Hydrochloride

HRID 856771ノート

反応式

HRID 856771 の反応式
[CH2:1]([N:3]1[C:7]([CH2:8]O)=[CH:6][N:5]=[CH:4]1)[CH3:2].S(Cl)([Cl:12])=O>>[ClH:12].[Cl:12][CH2:8][C:7]1[N:3]([CH2:1][CH3:2])[CH:4]=[N:5][CH:6]=1

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 22988641(1-Ethyl-1H-imidazol-5-yl)methanol

生成物 1

HCID 229387405-(Chloromethyl)-1-Ethyl-1H-Imidazole Hydrochloride

反応条件

温度
90 °C

実験手順

To 1-ethyl-5-hydroxymethylimidazole (9.5 g), thionyl chloride (50 ml) was added by portions at 0° C., and the mixture was heated for 30 minutes under nitrogen atmosphere at 90° C. The mixture was allowed to be at room temperature. The solvent was distilled off under reduced pressure and the obtained residue was dissolved in methanol, and the solvent was distilled off again under reduced pressure. The obtained solid was recrystallized from ethyl acetate, to give 5-chloromethyl-1-ethylimidazole hydrochloride (12.4 g) as colorless crystals.

後処理

  1. customto be at room temperature
  2. distillationThe solvent was distilled off under reduced pressure
  3. dissolutionthe obtained residue was dissolved in methanol
  4. distillationthe solvent was distilled off again under reduced pressure
  5. customThe obtained solid was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-230b7f53409948d0b950c5669e97b5db
出典データセット
uspto-grants-2007_08
特許番号
US07262185B2

反応ノート

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