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3-ethoxycarbonylmethyl-6-fluoro-5-nitro-2(3H)-benzothiazolone → 5-amino-3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-ethoxycarbonylmethyl-6-fluoro-5-nitro-2(3H)-benzothiazolone | HCID 14014244 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-amino-3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolone | HCID 14014245 | 71.7% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04888428 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-74511024267542968a8c318fedce1e25 |
| 出典メモ | uspto-grants-1989_12 |