Phosphorus oxybromide → HCID 19381666、化合物
反応式
[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]=1参加物
4
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-274063bdc9ee490884458502300f3089
- 出典データセット
- uspto-grants-1995_10
- 特許番号
- US05455348
反応ノート
読み込み中…