HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-ethoxycarbonylmethyl-6-fluoro-5-nitro-2(3H)-benzothiazolone → 5-amino-3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-ethoxycarbonylmethyl-6-fluoro-5-nitro-2(3H)-benzothiazolone | HCID 14014244 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 5-amino-3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolone | HCID 14014245 | 71.7% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04888428 |
| Source dataset | uspto-grants-1989_12 |
| ORD ID | ord-74511024267542968a8c318fedce1e25 |
| Source note | uspto-grants-1989_12 |