Thionyl Chloride → HCID 23076585、化合物
反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([CH2:8]O)[N:5]=[CH:4]1)[CH3:2].S(Cl)([Cl:12])=O>O1CCCC1>[ClH:12].[Cl:12][CH2:8][C:6]1[N:5]=[CH:4][N:3]([CH2:1][CH3:2])[CH:7]=1参加物
4
実験手順
To a solution (100 mL) of (1-ethyl-1H-imidazol-4-yl)methanol (5.80 g) in tetrahydrofuran was added thionyl chloride (14.59 g). The reaction mixture was heated under reflux for 1 hr and concentrated. Diethyl ether was added to the residue to allow crystallization, and the obtained crystals were collected by filtration, and washed with diethyl ether. The obtained crystals were recrystallized from methanol-tetrahydrofuran to give 4-chloromethyl-1-ethyl-1H-imidazole hydrochloride as colorless crystals (8.35 g, yield 100%).
後処理
- temperatureThe reaction mixture was heated
- temperatureunder reflux for 1 hr
- concentrationconcentrated
- additionDiethyl ether was added to the residue
- customcrystallization
- filtrationthe obtained crystals were collected by filtration
- washwashed with diethyl ether
- customThe obtained crystals were recrystallized from methanol-tetrahydrofuran
出典と根拠
- ORDレコード
- ord-09d422aada6a43968ca6a817561fbaf9
- 出典データセット
- uspto-grants-2008_05
- 特許番号
- US07368578B2
反応ノート
読み込み中…