Phosphorus oxybromide → HCID 19381666, 화합물
반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]=[CH:11][C:12](=O)[NH:13][CH:14]=2)=[CH:5][CH:4]=1.P(Br)(Br)([Br:18])=O>O>[Br:18][C:12]1[CH:11]=[N:10][C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[CH:14][N:13]=1참가 물질
4
실험 절차
26.1 g of 5-(4-methoxyphenyl)-2(1H)pyrazinone and 140 g of phosphorusoxybromide are heated to 100° C. for 45 minutes. After cooling, the hardened mass is added in batches to ice and water, with stirring. After 30 minutes stirring the mixture is left to stand for 18 hours and the precipitate is suction filtered. The filtrate is extracted with methylene chloride and the precipitate is dissolved in methylene chloride extract. The methylene chloride solution is washed with sodium bicarbonate solution, dried, filtered over activated charcoal and evaporated down.
후처리
- temperatureAfter cooling
- stirringAfter 30 minutes stirring the mixture
- waitis left
- filtrationfiltered
- extractionThe filtrate is extracted with methylene chloride
- dissolutionthe precipitate is dissolved in methylene chloride
- extractionextract
- washThe methylene chloride solution is washed with sodium bicarbonate solution
- customdried
- filtrationfiltered over activated charcoal
- customevaporated down
출처 및 근거
- ORD 기록
- ord-274063bdc9ee490884458502300f3089
- 출처 데이터셋
- uspto-grants-1995_10
- 특허 번호
- US05455348
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