2-hydroxy-N,N-dimethyl-3-nitrobenzamide → 3-Amino-2-hydroxy-N,N-dimethylbenzamide
反応式
[OH:1][C:2]1[C:12]([N+:13]([O-])=O)=[CH:11][CH:10]=[CH:9][C:3]=1[C:4]([N:6]([CH3:8])[CH3:7])=[O:5].[H][H]>C(O)C.[Pd]>[NH2:13][C:12]1[C:2]([OH:1])=[C:3]([CH:9]=[CH:10][CH:11]=1)[C:4]([N:6]([CH3:8])[CH3:7])=[O:5]参加物
5
実験手順
A solution of 33.5 g of 2-hydroxy-N,N-dimethyl-3-nitrobenzamide in 600 ml of ethanol were added to a suspension of 3.35 g of Pd/C 10% in 70 ml of ethanol. The reaction medium was stirred under 2 bar of hydrogen overnight. TLC and HPLC control (t=0.66 M+181). The reaction medium was filtered through celite and the filtrate was evaporated. 29 g of 3-amino-2-hydroxy-N,N-dimethylbenzamide were obtained in the form of an oily brown solid. Yield=100%.
後処理
- filtrationThe reaction medium was filtered through celite
- customthe filtrate was evaporated
出典と根拠
- ORDレコード
- ord-1f305bcd9200474aaa6f7fab72f24f46
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09090596B2
反応ノート
読み込み中…