反応式
[Br:1][CH2:2][C:3]1([CH3:25])[CH:7]([C:8]([OH:10])=[O:9])[N:6]2[C:11](=[O:24])[CH:12]([NH:13][C:14](=[O:23])[CH2:15][O:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C@H:5]2[S:4]1.[OH:26]O>C(O)(=O)C.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[Br:1][CH2:2][C:3]1([CH3:25])[CH:7]([C:8]([OH:10])=[O:9])[N:6]2[C:11](=[O:24])[CH:12]([NH:13][C:14](=[O:23])[CH2:15][O:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[C@H:5]2[S:4]1=[O:26]参加物
実験手順
Sodium tungstate (0.02 g) was added to a solution of 2-bromomethyl-2-methyl-6-(2-phenoxyacetamido)penam-3-carboxylic acid (3.1 g) in acetic acid (8 ml) at 7°-10° C under stirring and then to the mixture was added 30% aqueous hydrogen peroxide (1.2 ml). The mixture was stirred at 7°-10° C for 1 hour. After the reaction, ice-water (50 ml) was added to the reaction mixture and then extracted with ethyl acetate. The extract was washed with water and back-extracted with 5% sodium bicarbonate aqueous solution. The aqueous layer was washed with ethyl acetate twice, acidified with 5% hydrochloric acid to pH2 and then extracted with ethyl acetate. The extract was washed with water, dried and concentrated to give powder of 2-bromomethyl-2-methyl-6-(2-phenoxyacetamido)penam-3-carboxylic acid-1-oxide (2 g).
後処理
- stirringThe mixture was stirred at 7°-10° C for 1 hour
- additionwas added to the reaction mixture
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- extractionback-extracted with 5% sodium bicarbonate aqueous solution
- washThe aqueous layer was washed with ethyl acetate twice
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-ffe173b7c8de42b09a0f8ac7cab35e36
- 出典データセット
- uspto-grants-1977_11
- 特許番号
- US04056521
関連ノート
読み込み中…