Acetone → 1-Chloro-2-(5,6-dichloro-1-methyl-1H-benzoimidazol-2-yl)-propan-2-ol
反応式
[Cl:1][C:2]1[C:14]([Cl:15])=[CH:13][C:5]2[N:6]([CH3:12])[C:7](C(C)=C)=[N:8][C:4]=2[CH:3]=1.[Cl:16]N1C(=O)N(Cl)C(=O)N(Cl)C1=O.[CH3:28][C:29]([CH3:31])=[O:30]>O>[Cl:16][CH2:28][C:29]([C:7]1[N:6]([CH3:12])[C:5]2[CH:13]=[C:14]([Cl:15])[C:2]([Cl:1])=[CH:3][C:4]=2[N:8]=1)([OH:30])[CH3:31]参加物
5
実験手順
To 5,6-dichloro-1-methyl-2-isopropenyl-1H-benzimidazole (2.5 g) in acetone (30 mL) and water (6 mL) at room temperature was added trichloroisocyanuric acid (845 mg). The resulting mixture was stirred at room temperature for 18 h. The reaction mixture was quenched with water, extracted with EtOAc, and dried over Na2SO4. After removal of the desiccant by filtration, concentration yielded an orange crude oil. The crude product was purified by flash chromatography (10%-40% EtOAc/hexanes) to yield the title compound as a yellow solid.
後処理
- customThe reaction mixture was quenched with water
- extractionextracted with EtOAc
- dry with materialdried over Na2SO4
- customAfter removal of the
- filtrationdesiccant by filtration, concentration
- customyielded an orange crude oil
- customThe crude product was purified by flash chromatography (10%-40% EtOAc/hexanes)
出典と根拠
- ORDレコード
- ord-620baf2608d34dcebfdff9a4d3a7b287
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07879895B2
反応ノート
読み込み中…