Ammonium thiocyanate → HCID 22572976、化合物
反応式
[C:1]([C:5]1[CH:6]=[CH:7][C:8]([N+:12]([O-:14])=[O:13])=[C:9]([NH2:11])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[S-:15][C:16]#[N:17].[NH4+].BrBr>CO>[C:1]([C:5]1[C:6]([S:15][C:16]#[N:17])=[CH:7][C:8]([N+:12]([O-:14])=[O:13])=[C:9]([NH2:11])[CH:10]=1)([CH3:4])([CH3:2])[CH3:3]参加物
5
実験手順
The title compound was prepared according to the General Method 13 using 5-tert-butyl-2-nitro-phenylamine (prepared in Example PP-2; 170 g, 876 mmol), ammonium thiocyanate (400 g, 5260 mmol), bromine (140 g, 876 mmol), and MeOH (500 mL). The crude reaction mixture was purified by flash silica gel chromatography (5%-50% EtOAc in hexanes as eluents). MS(APCI): 252 (M+H).
後処理
- customThe crude reaction mixture
- customwas purified by flash silica gel chromatography (5%-50% EtOAc in hexanes as eluents)
出典と根拠
- ORDレコード
- ord-c3d67ade9bf444798c75e280e6f8169b
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852711B2
反応ノート
読み込み中…