HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2-[3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolon-5-yl]4,5,6,7-tetrahydro-2H-isoindole-1,3-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 3,4,5,6-Tetrahydrophthalic anhydride | HCID 12475 | — |
| Edukt | 5-amino-3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolone | HCID 14014245 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Produkt | 2-[3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolon-5-yl]4,5,6,7-tetrahydro-2H-isoindole-1,3-dione | HCID 14014246 | 19,1% |
Reaktionsschritte
5-Amino-3-ethoxycarbonylmethyl-6-fluoro-2(3H)benzothiazolone (140 mg) and 3,4,5,6-tetrahydrophthalic anhydride (90 mg) were suspended in acetic acid (3 ml), and the resultant suspension was heated under reflux for 5 hours. After being allowed to cool, water was added thereto, and the resultant mixture was extracted with ethyl acetate. The extract ws washed with water and sodium bicarbonte solution, dried and concentrated. The residue was purified by silica gel thin layer chromatography with a mixture of ethyl acetate and hexane (1:2) to give 2-[3-ethoxycarbonylmethyl-6-fluoro-2(3H)-benzothiazolon-5-yl]4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (40 mg). m.p., 155.5°-156.5° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04888428 |
| Quelldatensatz | uspto-grants-1989_12 |
| ORD ID | ord-6315777bab0346709ccb5beb232dceb4 |
| Quellennotiz | uspto-grants-1989_12 |