Ammonium Chloride → 1-benzyl-5-[4-(4-fluorophenyl)-1-hydroxy-1-(4-tert-butylaminocarbonylphenyl)butyl]-1-H-imidazole
反応式
[C:1]([NH:5][C:6]([C:8]1[CH:13]=[CH:12][C:11](Br)=[CH:10][CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([Li])CCC.[CH2:20]([N:27]1[C:31]([C:32](=[O:43])[CH2:33][CH2:34][CH2:35][C:36]2[CH:41]=[CH:40][C:39]([F:42])=[CH:38][CH:37]=2)=[CH:30][N:29]=[CH:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[Cl-].[NH4+]>O1CCCC1.CCCCCC>[CH2:20]([N:27]1[C:31]([C:32]([OH:43])([C:11]2[CH:12]=[CH:13][C:8]([C:6]([NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])=[CH:9][CH:10]=2)[CH2:33][CH2:34][CH2:35][C:36]2[CH:41]=[CH:40][C:39]([F:42])=[CH:38][CH:37]=2)=[CH:30][N:29]=[CH:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- -70 °C
実験手順
9,9 g of p-tert-butylaminocarbonylphenyl bromide is dissolved in 200 ml of dry tetrahydrofuran and cooled to -70° C. To the solution is added dropwise n-butyl lithium (5,3 g) in hexane and the mixture is stirred for one hour. 1-benzyl-5-[4-(4-fluorophenyl)-1-oxobutyl]-1H-imidazole (10,4 g) in 200 ml of tetrahydrofuran is added to the mixture at -70° C. and the mixture is allowed to warm to room temperature and stirring is continued over night. Saturated ammonium chloride is added to the mixture and the solution is extracted with ethyl acetate. Ethyl acetate fractions are combined and evaporated to dryness.
後処理
- temperatureto warm to room temperature
- stirringstirring
- waitis continued over night
- extractionthe solution is extracted with ethyl acetate
- customevaporated to dryness
出典と根拠
- ORDレコード
- ord-3d543c7ead7d4e2db77bbcedf9e71a6c
- 出典データセット
- uspto-grants-1996_09
- 特許番号
- US05559141
反応ノート
読み込み中…