反応式
[CH:1]([O:4][C:5]([C:7]1[CH:8]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([N+:25]([O-:27])=[O:26])[CH:20]=2)[C:9]2[C:14](=[O:15])[NH:13][CH:12]=[N:11][C:10]=2[NH:16][C:17]=1[CH3:18])=[O:6])([CH3:3])[CH3:2].[CH3:28][O+](C)C.F[B-](F)(F)F>ClCCCl>[CH:1]([O:4][C:5]([C:7]1[CH:8]([C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([N+:25]([O-:27])=[O:26])[CH:20]=2)[C:9]2[C:14]([O:15][CH3:28])=[N:13][CH:12]=[N:11][C:10]=2[NH:16][C:17]=1[CH3:18])=[O:6])([CH3:3])[CH3:2]参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
Three and 0.7 g (10 mmol) (±)-3,4,5,8-tetrahydro-7-methyl-5-(3-nitrophenyl)-4-oxo-pyrido[2,3-d]-pyrimidine-6-carboxylic acid isopropyl ester and 3.0 g (20 mmol) trimethyloxonium-tetrafluoroborate are stirred in 150 ml 1,2-dichloroethane in nitrogen atmosphere and at room temperature for three hours. The product is extracted twice with 50 ml saturated sodium hydrogen carbonate solution, the organic phase is separated, dried over sodium sulfate and reduced under vacuum. Twice recrystallizing the residue from diisopropyl ether/isopropanol yields the product in the form of colorless crystals with a mp of 212°-213° C.
後処理
- extractionThe product is extracted twice with 50 ml saturated sodium hydrogen carbonate solution
- customthe organic phase is separated
- dry with materialdried over sodium sulfate
- customTwice recrystallizing the residue from diisopropyl ether/isopropanol
- customyields the product in the form of colorless crystals with a mp of 212°-213° C.
出典と根拠
- ORDレコード
- ord-e09c11473fef44f999758252a4e6c990
- 出典データセット
- uspto-grants-1988_08
- 特許番号
- US04762837
関連ノート
読み込み中…