Thiophosgene → 1,3-Dibromo-2-isothiocyanato-5-methoxybenzene
反応式
[C:1](Cl)(Cl)=[S:2].[Br:5][C:6]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[C:9]([Br:15])[C:7]=1[NH2:8]>O1CCCC1.C(=O)([O-])O.[Na+]>[Br:5][C:6]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[C:9]([Br:15])[C:7]=1[N:8]=[C:1]=[S:2]参加物
5
実験手順
Thiophosgene (1.52 mL, 20.5 mmol) was added dropwise to a stirred mixture of 2,6-dibromo-4-methoxyaniline (2.86 g, 10.2 mmol) in tetrahydrofuran (25 mL) and saturated aqueous sodium hydrogen carbonate (25 mL) at 0° C. The mixture was stirred at room temperature for 1 h, and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give the title compound as a yellow solid (3.22 g, 9.97 mmol, 98%).
後処理
- extractionextracted with ethyl acetate
- washThe combined organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-dd3b2779e22947d08db5c9d35df5a064
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08901141B2
反応ノート
読み込み中…