Methyl iodide → 5,6-Difluoro-2-(methylsulfanyl)-1,3-benzothiazole
反応式
[F:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[S:9][C:8]([SH:10])=[N:7][C:6]=2[CH:11]=1.[C:13](=O)([O-])[O-].[K+].[K+].IC>CN(C)C=O.O>[F:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[S:9][C:8]([S:10][CH3:13])=[N:7][C:6]=2[CH:11]=1参加物
6
反応条件
- 温度
- 0 °C
実験手順
A suspension (0° C.) of 300 mg (1.476 mmol) 5,6-difluoro-benzothiazole-2-thiol and 306 mg (2.214 mmol) potassium carbonate in 6 mL N,N-dimethylformamide under nitrogen, were added 110.5 μL (1.77 mmol) iodomethane. The mixture was stirred at 0° C. for 1 h. The mixture was diluted with water (30 mL) and extracted with ethyl acetate. The combined extracts were washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo to provide 294 mg (91.7%) of the title compound as a solid. MS(m/e): 218.3 (M+H+).
後処理
- extractionextracted with ethyl acetate
- washThe combined extracts were washed with water and brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-42fff5004a39426cbcdd2fc6075afefb
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07897627B2
反応ノート
読み込み中…