HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 7-Chloro-3-[[(isopropylamino)oxy]carbonyl]pyrazolo[3,4-c]-[1]benzazepine-4,10(1H,9H)-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Edukt | N-Isopropylhydroxylamine Hydrochloride | HCID 170873 | — |
| Edukt | HCID 178524941 | HCID 178524941 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 7-Chloro-3-[[(isopropylamino)oxy]carbonyl]pyrazolo[3,4-c]-[1]benzazepine-4,10(1H,9H)-dione | HCID 178458085 | 47% |
Reaktionsschritte
A solution of 7-chloro-3-(carboxy)pyrazolo[3,4-c][1]-benzazepine-4,10(1H,9H)-dione (300 mg, 1.03 mmol) (compound of Example 9) and 1,1′-carbonyldiimidazole (251 mg, 1.55 mmol) in N,N-dimethylformamide (12 mL) was stirred for 1 hour. In one portion N-isopropylhydroxylamine hydrochloride (345 mg, 3.09 mmol) was added and the solution was stirred for 55 minutes at room temperature. To the resulting solution was added water (40 mL) giving a precipitate which was separated by filtration. This Crude product was purified by flash chromatography eluting with chloroform:2-propanol (98:2-96.5:3.5) to give the title compound (167 mg, 47% yield, m.p. 224° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06313290B1 |
| Quelldatensatz | uspto-grants-2001_11 |
| ORD ID | ord-780dac8daad9411cbd47cf46b31228b0 |
| Quellennotiz | uspto-grants-2001_11 |