Methanesulfonyl chloride → 2-(chloro(5-ethoxy-2-fluoro-3-isopropoxyphenyl)methyl)-4-phenyl-1-trityl-1H-imidazole
反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([O:43][CH:44]([CH3:46])[CH3:45])[C:7]([F:42])=[C:8]([CH:10]([C:12]2[N:13]([C:23]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:14]=[C:15]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[N:16]=2)O)[CH:9]=1)[CH3:2].CS([Cl:51])(=O)=O>C(Cl)Cl.CN(C1C=CN=CC=1)C.CCOC(C)=O>[Cl:51][CH:10]([C:8]1[CH:9]=[C:4]([O:3][CH2:1][CH3:2])[CH:5]=[C:6]([O:43][CH:44]([CH3:46])[CH3:45])[C:7]=1[F:42])[C:12]1[N:13]([C:23]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:14]=[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:16]=1参加物
6
反応物 2
生成物 1
試薬・触媒・溶媒 3
実験手順
To a solution of Intermediate 25.1 (100 mg, 0.163 mmol) in 2 mL CH2Cl2, were added DMAP (2 mg, cat.), TEA (27 μL, 0.20 mmol) and MsCl (15.2 μL, 0.196 mmol). The mixture was stirred at rt for 30 min, then TEA (27 μL, 0.20 mmol) and MsCl (15.2 μL, 0.196 mmol) were added. The mixture was stirred at rt for 30 min, then was diluted with EtOAc, washed with H2O and brine, dried (Na2SO4) and concentrated. to afford 125 mg of Intermediate 25.2 as a yellow solid, which was used in the following step without further purification.
後処理
- stirringThe mixture was stirred at rt for 30 min
- washwashed with H2O and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-af4f2bb0a4604ea5bf3dd15e8b88d870
- 出典データセット
- uspto-grants-2009_08
- 特許番号
- US07576098B2
反応ノート
読み込み中…