Sodium Hydroxide → (2,4-Dichloro-3-nitrophenyl)methanamine
反応式
[N+:1]([C:4]1[C:5]([Cl:19])=[C:6]([CH:15]=[CH:16][C:17]=1[Cl:18])[CH2:7][NH:8]C(=O)C(F)(F)F)([O-:3])=[O:2].[OH-].[Na+]>CO>[N+:1]([C:4]1[C:5]([Cl:19])=[C:6]([CH:15]=[CH:16][C:17]=1[Cl:18])[CH2:7][NH2:8])([O-:3])=[O:2]参加物
4
実験手順
A mixture of N-(3-nitro-2,4-dichloro-benzyl)-2,2,2-trifluoroacetamide (0.66 g, impure, content ˜50%), 4M NaOH-solution (1.3 mL, 5.2 mmol) and MeOH (15 mL) is refluxed for 4 h. Then the mixture is concentrated, diluted with water, acidified with 4M HCl, filtered, 4M NaOH-solution is added and it is extracted with EtOAc. The organic phase is dried with Na2SO4, filtered and concentrated. Yield 0.17 g
後処理
- temperatureis refluxed for 4 h
- concentrationThen the mixture is concentrated
- additiondiluted with water
- filtrationfiltered
- addition4M NaOH-solution is added
- extractionit is extracted with EtOAc
- dry with materialThe organic phase is dried with Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9cc292976eae4befa2ee1517a8bd3287
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08759537B2
反応ノート
読み込み中…