Thionyl Chloride → HCID 22938531、化合物

反応式

O[CH2:2][C:3]1[N:7]([CH:8]([CH3:10])[CH3:9])[CH:6]=[N:5][CH:4]=1.S(Cl)([Cl:13])=O>>[ClH:13].[Cl:13][CH2:2][C:3]1[N:7]([CH:8]([CH3:10])[CH3:9])[CH:6]=[N:5][CH:4]=1

参加物

反応物 2

HCID 24386Thionyl Chloride

HCID 20568531(1-(propan-2-yl)-1H-imidazol-5-yl)methanol

生成物 1

HCID 22938531HCID 22938531、化合物

反応条件

温度: 90 °C

実験手順

To 5-hydroxymethyl-1-isopropylimidazole (4.5 g), thionyl chloride (20 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-isopropylimidazole hydrochloride (6.2 g) as colorless crystals.

後処理

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

出典と根拠

ORDレコード: ord-22215d6b82654220bea74dff3256e168
出典データセット: uspto-grants-2007_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07262185B2

反応ノート

読み込み中…

参加物