Sodium methanethiolate → HCID 86701454、化合物
反応式
Br[C:2]1[CH:9]=[C:8]([CH3:10])[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][C:3]=1[C:4]#[N:5].[CH3:14][S-:15].[Na+]>CN(C=O)C>[CH3:10][C:8]1[C:7]([N+:11]([O-:13])=[O:12])=[CH:6][C:3]([C:4]#[N:5])=[C:2]([S:15][CH3:14])[CH:9]=1参加物
4
反応条件
- 温度
- 60 °C
実験手順
To a solution of 2-bromo-4-methyl-5-nitrobenzonitrile (3 g, 12.45 mmol) in DMF (124 mL), sodium thiomethoxide (1.31 g, 18.67 mmol) was added and the reaction heated to 60° C. for 1 h. The reaction was then cooled to room temperature, quenched with a sat. aq. solution of NaHCO3 and extracted with EtOAc. The organic extract was dried over MgSO4, filtered and concentrated. The resulting residue was purified using FCC eluting with heptanes:EtOAc 1:1 to give the title compound. MS (ESI−) m/z 207.3 (M−H).
後処理
- temperatureThe reaction was then cooled to room temperature
- customquenched with a sat. aq. solution of NaHCO3
- extractionextracted with EtOAc
- extractionThe organic extract
- dry with materialwas dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe resulting residue was purified
- washeluting with heptanes:EtOAc 1:1
出典と根拠
- ORDレコード
- ord-c8d07fd8bcaf459cb4b1a7ed276bb1e9
- 出典データセット
- uspto-grants-2015_06
- 特許番号
- US09056874B2
反応ノート
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