2-Methylbenzimidazole → 2-Methyl-1-propyl-1H-benzimidazole
反応式
[CH3:1][C:2]1[NH:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[H-].[Na+].I[CH2:14][CH2:15][CH3:16]>O1CCCC1>[CH3:1][C:2]1[N:6]([CH2:14][CH2:15][CH3:16])[C:5]2[CH:7]=[CH:8][CH:9]=[CH:10][C:4]=2[N:3]=1参加物
5
実験手順
To a flask were added 2.0 g 2-methylbenzimidazole and 40 ml tetrahydrofuran and the mixture was cooled to 10 C under nitrogen. 0.9 g Sodium hydride were added in portions and the reaction mixture was stirred for 20 minutes. 3.9 g 1-iodopropane were added and the mixture was heated to 45 C for 6 hours. The mixture was quenched slowly with 40 ml water, extracted twice with ethyl acetate and washed with water. Following solvent removal, the product was purified by silica gel chromatography using pure ethyl acetate to 5% methanol in ethyl acetate. A pale yellow oil was obtained.
後処理
- temperaturethe mixture was cooled to 10 C under nitrogen
- temperaturethe mixture was heated to 45 C for 6 hours
- customThe mixture was quenched slowly with 40 ml water
- extractionextracted twice with ethyl acetate
- washwashed with water
- customFollowing solvent removal
- customthe product was purified by silica gel chromatography
- customA pale yellow oil was obtained
出典と根拠
- ORDレコード
- ord-c3a183dfbad9400eb21fe4896878885c
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08431045B2
反応ノート
読み込み中…