Ammonium Chloride → 2-Amino-4-methoxy-5-(2-methoxyethoxy)benzamide
反応式
[CH3:1][O:2][C:3]1[C:11]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[CH:10][C:6]([C:7]([NH2:9])=[O:8])=[C:5]([N+:17]([O-])=O)[CH:4]=1.[NH4+].[Cl-]>COCCOC.CO.[Pd]>[NH2:17][C:5]1[CH:4]=[C:3]([O:2][CH3:1])[C:11]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[CH:10][C:6]=1[C:7]([NH2:9])=[O:8]参加物
6
実験手順
A mixture of 4-methoxy-5-(2-methoxyethoxy)-2-nitrobenzamide (4.5 g, contains some NH4Cl) and 10% Pd/C (ca. 0.5 g) in DME (200 mL) and MeOH (200 mL) was hydrogenated under a balloon of H2 at RT for 12 h. The mixture was filtered through a pad of Celite® and concentrated in vacuo to give 2-amino-4-methoxy-5-(2-methoxyethoxy)benzamide as an off white solid (2.8 g, 11.6 mmol). HPLC retention time 2.80 mins.
後処理
- filtrationThe mixture was filtered through a pad of Celite®
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-913498b9905e4b64a8d0d4341cb29da1
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08916576B2
反応ノート
読み込み中…