Ammonium Hydroxide → 2-Amino-5-methanesulfonylbenzoic acid
반응식
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]참가 물질
4
반응 조건
- 온도
- 127.5 °C
실험 절차
A mixture of 4.26 mmol 2-chloro-5-methanesulfonyl-benzoic acid (example B1a)), step1), 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 1 N 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%)
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-9b5b83baf20949e5b4faf859fb9c208e
- 출처 데이터셋
- uspto-grants-2009_07
- 특허 번호
- US07557114B2
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