反応式
[CH2:1]([O:3][C:4]([CH2:6][N:7]1[C:11]2[CH:12]=[C:13]([N+:17]([O-])=O)[C:14]([F:16])=[CH:15][C:10]=2[S:9][C:8]1=[O:20])=[O:5])[CH3:2]>C(O)(=O)C.C(OCC)(=O)C.[Fe]>[NH2:17][C:13]1[C:14]([F:16])=[CH:15][C:10]2[S:9][C:8](=[O:20])[N:7]([CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5])[C:11]=2[CH:12]=1参加物
5
実験手順
Electrolytic iron powder (0.29 g) was suspended in 5% acetic acid (2 ml), and a solution of 3-ethoxycarbonylmethyl-6-fluoro-5-nitro-2(3H)-benzothiazolone (0.31 g) in acetic acid (1 ml) and ethyl acetate (1 ml) was dropwise added thereto while heating. The resultant mixture was heated under reflux for 3 hours. The reaction mixture was subjected to filtration with celite, and the filtrate was extracted with ethyl acetate. The extract was washed with water and sodium bicarbonate solution, dried and concentrated to give 0.20 g of 5-amino-3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolone. m.p., 172.5°-173.5° C.
後処理
- temperaturewhile heating
- temperatureunder reflux for 3 hours
- filtrationThe reaction mixture was subjected to filtration with celite
- extractionthe filtrate was extracted with ethyl acetate
- washThe extract was washed with water and sodium bicarbonate solution
- customdried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-74511024267542968a8c318fedce1e25
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04888428
関連ノート
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