Water → 4-chloro-N-amino-phthalimide
반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[O:10])[NH:8][C:6](=[O:7])[C:5]2=[CH:11][CH:12]=1.O.[NH2:14]N.O>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[O:10])[N:8]([NH2:14])[C:6](=[O:7])[C:5]2=[CH:11][CH:12]=1참가 물질
5
실험 절차
To a cooled mixture of 1.81 g (10 mmol) 4-chloro phthalimide in 20 mL ethanol (96%) was added 0.5 mL (10 mmol) hydrazine monohydrate. The reaction mixture was stirred for 2 min. at room temperature and 2 min. at reflux. By adding 50 mL cold water pale yellow crystals formed alter 1 h. Resulting crystals was filtered and recrystallized from ethanol to give 0.4 g (20%) 4-chloro-N-amino-phthalimide: mp 172°-175° C.; 1H NMR (200 MHz, DMSO-d6) d 4.90 (s, 2H, NH2), 7.82-7.92 (m, 3H, C6H3); it solidifies after melting and melts again around 345° C.
후처리
- temperatureat reflux
- customformed
- waitalter 1 h
- customResulting crystals
- filtrationwas filtered
- customrecrystallized from ethanol
출처 및 근거
- ORD 기록
- ord-dc13ec50a9a2498396c2c96dfbba4e5e
- 출처 데이터셋
- uspto-grants-1994_10
- 특허 번호
- US05359092
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