반응식
[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]참가 물질
6
반응물 4
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 60 °C
실험 절차
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%).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-2c64f644d0a140b499da6f8248d16245
- 출처 데이터셋
- uspto-grants-2007_09
- 특허 번호
- US07268145B2
연결된 노트
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