反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9][C:10]2[N:14]([CH3:15])[C:13]([CH2:16][OH:17])=[N:12][C:11]=2[CH:18]([CH3:20])[CH3:19])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[NH+]1C=CC=CC=1.C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH3:38][O:39][C:40]1[CH2:45][CH2:44][CH2:43][CH2:42][CH:41]=1.C(N(CC)CC)C>C1(C)C=CC=CC=1>[Cl:8][C:6]1[CH:5]=[C:4]([S:9][C:10]2[N:14]([CH3:15])[C:13]([CH2:16][O:17][C:40]3([O:39][CH3:38])[CH2:45][CH2:44][CH2:43][CH2:42][CH2:41]3)=[N:12][C:11]=2[CH:18]([CH3:20])[CH3:19])[CH:3]=[C:2]([Cl:1])[CH:7]=1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-2-hydroxymethyl-1H-imidazole (14) (33 mg, 0.1 mmol) prepared in accordance with the method as described in WO 96/10019 and p-toluenesulfonic acid pyridinium (27.6 mg, 0.11 mmol) in toluene (1.5 mL) was added 1-methoxycyclohexene (112 mg, 1.00 mmol) under ice-cooling, and stirred at room temperature for 6 hours. A drop of triethylamine was added to the reaction mixture, and the mixture was filtered to remove the insoluble matter. The filtrate was concentrated under reduced pressure. The residue was purified by chromatography on an alumina column (eluate: toluene) to give the compound 15 (37.0 mg, 70%) as oil. Rf 0.16 (Al2O3 60, Type E, toluene).
後処理
- temperaturecooling
- filtrationthe mixture was filtered
- customto remove the insoluble matter
- concentrationThe filtrate was concentrated under reduced pressure
- customThe residue was purified by chromatography on an alumina column (eluate: toluene)
出典と根拠
- ORDレコード
- ord-a286971f7e184e91b02b73dd4c884107
- 出典データセット
- uspto-grants-2000_04
- 特許番号
- US06054591
関連ノート
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