反応式
[CH3:1][N:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=C(C=O)[C:17]=3[CH:23]=2)[C:3]1=[O:24].[CH:25]([SH:28])([SH:27])[CH3:26].B(F)(F)F.[CH3:33][CH2:34]OCC>C(Cl)Cl>[S:27]1[CH2:34][CH2:33][S:28][CH:25]1[C:26]1[C:17]2[CH:23]=[C:13]([N:4]3[C:5](=[O:12])[CH:6]=[C:7]([C:8]([F:9])([F:11])[F:10])[N:2]([CH3:1])[C:3]3=[O:24])[CH:14]=[CH:15][C:16]=2[S:20][N:19]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a mixture of 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-carboxaldehyde (0.300 g, 0.850 mmol) and methylene chloride is added ethanedithiol (0.0940 g, 1.00 mmol) and boron trifluoride-etherate (0.200 ml). The resultant mixture is stirred overnight at room temperature and partitioned between methylene chloride and saturated sodium bicarbonate. The organic layer is dried over anhydrous magnesium sulfate and concentrated in vacuo to a yellow solid which is stirred in hot methylcyclohexane and filtered to afford the title compound as a light yellow solid (0.170 g, 46.3%, mp 227-232° C.) which is identified by NMR spectral analysis.
後処理
- custompartitioned between methylene chloride and saturated sodium bicarbonate
- dry with materialThe organic layer is dried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo to a yellow solid which
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-8bf089df8a384e13a27e826f43e36cc3
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06706663B2
関連ノート
読み込み中…