Dimethylformamide → (5-methyl-1H-imidazol-4-yl)methyl[4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidin-2yl]formamide
反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[C:15]([C:17]([F:20])([F:19])[F:18])[N:14]=[C:13]([NH:21][CH:22]=[O:23])[N:12]=2)=[CH:7][CH:6]=1)(=[O:4])=[O:3].[H-].[Na+].Cl.Cl[CH2:28][C:29]1[N:30]=[CH:31][NH:32][C:33]=1C.[CH3:35]N(C)C=O>>[CH3:28][C:29]1[NH:30][CH:31]=[N:32][C:33]=1[C:22]([N:21]([CH3:35])[C:13]1[N:12]=[C:11]([C:8]2[CH:9]=[CH:10][C:5]([S:2]([CH3:1])(=[O:3])=[O:4])=[CH:6][CH:7]=2)[CH:16]=[C:15]([C:17]([F:19])([F:20])[F:18])[N:14]=1)=[O:23]参加物
5
反応物 4
生成物 1
実験手順
To a stirred solution of 4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidin-2-ylformamide (0.5 g, 1.54 mmol) in dry dimethylformamide (10 ml) under N2 was added sodium hydride (60% dispersion in oil, 0.16 g). The mixture was stirred for 30 mins, 4-(chloromethyl)-5-methyl-1H-imidazole, hydrochloride (0.283 g) was added and stirring was then continued at room temp for 18 h. The mixture was then partitioned between water and ethyl acetate. The extracts were dried (Na2SO4) and evaporated. The residue was then triturated with diethyl ether giving the crude title compound as a pale yellow solid (0.27 g).
後処理
- stirringstirring
- waitwas then continued at room temp for 18 h
- customThe mixture was then partitioned between water and ethyl acetate
- dry with materialThe extracts were dried (Na2SO4)
- customevaporated
- customThe residue was then triturated with diethyl ether giving the crude title compound as a pale yellow solid (0.27 g)
出典と根拠
- ORDレコード
- ord-a7b13d90e138458ca8cefda020f17ec7
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06780870B2
反応ノート
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