Methylamine → 2-Chloro-4-(methylamino)-5-nitrobenzonitrile
反応式
[CH3:1][NH2:2].[Cl:3][C:4]1[CH:11]=[C:10](F)[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][C:5]=1[C:6]#[N:7]>C1COCC1>[Cl:3][C:4]1[CH:11]=[C:10]([NH:2][CH3:1])[C:9]([N+:13]([O-:15])=[O:14])=[CH:8][C:5]=1[C:6]#[N:7]参加物
4
反応条件
- 温度
- -20 °C
実験手順
A solution of MeNH2 in THF (14.9 mL, 2 M, 29.8 mmol) was added dropwise to a solution of 2-chloro-4-fluoro-5-nitrobenzonitrile (3.0 g, 15 mmol) in THF (100 mL) at −20° C. The mixture was stirred at −20° C. for 1 h and thereafter concentrated, washed with brine and extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The resulting residue was washed with PE to give the sub-title compound.
後処理
- concentrationconcentrated
- washwashed with brine
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- washThe resulting residue was washed with PE
出典と根拠
- ORDレコード
- ord-f1119eec4ec94833850b30c3926a1f5a
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08466186B2
反応ノート
読み込み中…