Water → (3-Nitrobenzyl)(propyl)sulfane
反応式
Cl[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[CH:4]=1.[CH2:12]([S-:15])[CH2:13][CH3:14].[Na+].O>CN(C=O)C>[N+:9]([C:5]1[CH:4]=[C:3]([CH:8]=[CH:7][CH:6]=1)[CH2:2][S:15][CH2:12][CH2:13][CH3:14])([O-:11])=[O:10]参加物
5
反応条件
- 温度
- 60 °C
実験手順
A solution of 1-(chloromethyl)-3-nitrobenzene (10.0 g, 58.1 mmol) in DMF (30 mL) was stirred at room temperature, then sodium propane-1-thiolate (5.7 g, 58.1 mmol) was added, followed by stirring at 60° C. overnight. After water was added, the aqueous layer was extracted with ethyl acetate 3 times. The combined organic phase was washed with brine, dried over sodium sulfate and concentrated to give (3-nitrobenzyl)(propyl)sulfane (11.2 g, yield 91%).
後処理
- extractionthe aqueous layer was extracted with ethyl acetate 3 times
- washThe combined organic phase was washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-3f06213bfa9f4e0b9899ac993d41d6e2
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08461134B2
反応ノート
読み込み中…