Nitric Acid → HCID 178434486, 화합물
반응식
Br[C:2]1[C:3]([CH3:8])=[N:4][NH:5][C:6]=1[Br:7].[N+:9]([O-])([OH:11])=[O:10].O>S(=O)(=O)(O)O>[Br:7][C:6]1[NH:5][N:4]=[C:3]([CH3:8])[C:2]=1[N+:9]([O-:11])=[O:10]참가 물질
5
반응 조건
- 온도
- 9 °C
실험 절차
6.5 g (0.027 mole) of 4,5-dibromo-3-methylpyrazole was dissolved in 20 ml of concentrated sulfuric acid. The solution was cooled to 9° C. and 10 ml of 90% nitric acid was added dropwise. The solution was stirred 30 minutes and then slowly heated to 60° C. and kept at that temperature for 30 minutes. The solution was cooled and poured into water. The mixture was extracted with ether and the ether was washed with water. The ether solution, after drying over magnesium sulfate was concentrated in vacuo and gave a white solid (1.5 g). One recrystallization from ethyl acetate gave a solid product.
후처리
- temperatureslowly heated to 60° C.
- waitkept at that temperature for 30 minutes
- temperatureThe solution was cooled
- extractionThe mixture was extracted with ether
- washthe ether was washed with water
- dry with materialThe ether solution, after drying over magnesium sulfate
- concentrationwas concentrated in vacuo
출처 및 근거
- ORD 기록
- ord-4e336a0aba884b64a848a83567d9f284
- 출처 데이터셋
- uspto-grants-1977_05
- 특허 번호
- US04025530
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