Ammonium Hydroxide → 2-Amino-5-methanesulfonylbenzoic acid
反応式
Cl[C:2]1[CH:10]=[CH:9][C:8]([S:11]([CH3:14])(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[OH-].[NH4+:16]>[Cu]>[NH2:16][C:2]1[CH:10]=[CH:9][C:8]([S:11]([CH3:14])(=[O:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]参加物
4
反応条件
- 温度
- 127.5 °C
実験手順
A mixture of 4.26 mmol 2-chloro-5-methanesulfonyl-benzoic acid, 0.39 mmol Copper powder and 10 ml ammonium hydroxide 25% was heated at 125-130° C. with stirring for 18 hours. Mixture was cooled to room temperature and filtered. The solid was washed with methanol. The filtrate was concentrated in vacuo. The residue was acidified with HCl 1N to pH=2. The obtained solid was washed with water and dried (HV, 50° C., 1 hour) to yield the title compound. MS (m/e): 214.1 (M−H, 100%)
後処理
- temperatureMixture was cooled to room temperature
- filtrationfiltered
- washThe solid was washed with methanol
- concentrationThe filtrate was concentrated in vacuo
- washThe obtained solid was washed with water
- customdried (HV, 50° C., 1 hour)
出典と根拠
- ORDレコード
- ord-7674e59c41864e23b2c930727e93c1ff
- 出典データセット
- uspto-grants-2009_10
- 特許番号
- US07605163B2
反応ノート
読み込み中…