HCID 86701454、化合物 → HCID 86701455、化合物
反応式
[CH3:1][C:2]1[C:9]([N+:10]([O-])=O)=[CH:8][C:5]([C:6]#[N:7])=[C:4]([S:13][CH3:14])[CH:3]=1.[CH:15]([Mg]Br)=[CH2:16]>C1COCC1>[CH3:1][C:2]1[C:9]2[NH:10][CH:16]=[CH:15][C:8]=2[C:5]([C:6]#[N:7])=[C:4]([S:13][CH3:14])[CH:3]=1参加物
4
反応条件
- 温度
- -78 °C
実験手順
To a solution of 4-methyl-2-(methylthio)-5-nitrobenzonitrile (1.6 g, 7.68 mmol) in THF (80 mL) at −78° C. under nitrogen, was added rapidly 1M vinylmagnesium bromide in THF (30.7 mL, 30.7 mmol). After addition was complete, the reaction was stirred at −78° C. for 30 min. The reaction was then quenched with sat. aq. NH4Cl and extracted with EtOAc. The organic extract was dried over MgSO4, filtered and concentrated. The pure title compound was isolated using FCC (0-50% EtOAc in heptanes). MS (ESI−) m/z 201.2 (M−H).
後処理
- additionAfter addition
- customThe reaction was then quenched with sat. aq. NH4Cl
- extractionextracted with EtOAc
- extractionThe organic extract
- dry with materialwas dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-0fb2a24242004d4f9406620099e63a85
- 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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