反応式
[H-].[Na+].O1[CH2:7][CH2:6][CH2:5][CH2:4]1.[CH3:8][C:9]1[C:27]([CH3:28])=[CH:26][C:12]2[N:13]=[C:14]([S:16][CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[C:24]#[N:25])[NH:15][C:11]=2[CH:10]=1.Cl[C:30]1[CH:37]=CC(Cl)=[CH:34][C:31]=1[CH2:32]Cl>O>[CH3:4][C:5]1[CH:37]=[CH:30][C:31]([CH3:34])=[CH:32][C:6]=1[CH2:7][N:15]1[C:11]2[CH:10]=[C:9]([CH3:8])[C:27]([CH3:28])=[CH:26][C:12]=2[N:13]=[C:14]1[S:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[C:24]#[N:25]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 60 °C
実験手順
Sodium hydride (178 mg, 4.90 mmol) and tetrahydrofuran (30 ml) were added to a previously dried reaction vessel. To the mixture were added 2-((5,6-dimethylbenzimidazole-2-ylthio)methyl)benzenecarbonitrile (719 mg, 2.45 mmol) and 2,5-dichlorobenzyl chloride (543 μl, 4.90 mmol), and the mixture was stirred at 60° C. for 40 minutes. Water was added thereto, followed by extraction with ethyl acetate. After the ethyl acetate phase was dried with anhydrous sodium sulfate, it was concentrated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to obtain 2-((1-((2,5-dimethylphenyl)methyl)-5,6-dimethylbenzimidazole-2-ylthio)methyl)benzenecarbonitrile (370 mg, yield 37%).
後処理
- extractionfollowed by extraction with ethyl acetate
- dry with materialAfter the ethyl acetate phase was dried with anhydrous sodium sulfate, it
- concentrationwas concentrated
- customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)
出典と根拠
- ORDレコード
- ord-2c64f644d0a140b499da6f8248d16245
- 出典データセット
- uspto-grants-2007_09
- 特許番号
- US07268145B2
関連ノート
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