Hydrochloric Acid → HCID 178420123、化合物
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:8]=[CH:9][N:10](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[CH:11]=1.Cl>O1CCCC1>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[N:8]=[CH:9][NH:10][CH:11]=1参加物
4
実験手順
A solution of the crude 4-(2-pyridyl)-1-trityl-1H-imidazole (0.69g) in tetrahydrofuran (14 mL) was treated with 2 N hydrochloric acid (7.2 mL) and heated at reflux for 45 minutes. After cooling the reaction mixture was concentrated in vacuo and the residue was dissolved in dichloromethane (20 mL). The organic solution was successively washed with aqueous 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL). The organic solution was then dried over anhydrous sodium sulfate, filtered, and concentrated in-vacuo to afford 0.12 g of crude 4-(2-pyridyl)imidazole, as a sticky white solid.
後処理
- temperatureheated
- temperatureat reflux for 45 minutes
- temperatureAfter cooling the reaction mixture
- concentrationwas concentrated in vacuo
- dissolutionthe residue was dissolved in dichloromethane (20 mL)
- washThe organic solution was successively washed with aqueous 1N sodium hydroxide (10 mL), water (20 mL) and brine (20 mL)
- dry with materialThe organic solution was then dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in-vacuo
出典と根拠
- ORDレコード
- ord-53d968e1a3174d4f8f50d9e6161031f7
- 出典データセット
- uspto-grants-2003_12
- 特許番号
- US06660753B2
反応ノート
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