反応式
[F:1][C:2]([F:22])([F:21])[S:3]([NH:6][C:7]1[CH:20]=[CH:19][CH:18]=[CH:17][C:8]=1[CH2:9][N:10]1[CH2:15][CH2:14][CH2:13][O:12][C:11]1=[O:16])(=[O:5])=[O:4].C(=O)([O-])O.[Na+].Cl[C:29]([O:31][CH2:32][CH2:33][CH3:34])=[O:30].O>C(#N)C>[CH2:32]([O:31][C:29]([N:6]([C:7]1[CH:20]=[CH:19][CH:18]=[CH:17][C:8]=1[CH2:9][N:10]1[CH2:15][CH2:14][CH2:13][O:12][C:11]1=[O:16])[S:3]([C:2]([F:1])([F:21])[F:22])(=[O:5])=[O:4])=[O:30])[CH2:33][CH3:34]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
3-[2-(Trifluoromethanesulfonylamino)benzyl]-[1,3]-oxazinan-2-one (0.13 g, 0.38 mmol) and sodium hydrogen carbonate (0.06 g, 0.71 mmol) was suspended in acetonitrile (15 ml), added with propyl chloroformate (0.09 g, 0.77 mmol) and heated to reflux for six hours. After cooling to room temperature, the reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with a saturated brine and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4) to obtain 3-{2-[N-(propoxycarbonyl)-N-(trifluoromethanesulfonyl)amino]benzyl)-[1,3]-oxazinan-2-one (0.11 g).
後処理
- temperatureheated
- temperatureto reflux for six hours
- extractionextracted with ethyl acetate
- washThe organic layer was washed with a saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:4)
出典と根拠
- ORDレコード
- ord-6b8d7d689bc74860aaa9e3e40448eaac
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08048825B2
関連ノート
読み込み中…