HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropanol → HCID 178459484, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropanol | HCID 3776 | — |
| Reactant | 7-Chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10-(1H,9H)dione | HCID 178470481 | — |
| Catalyst | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 178459484 | HCID 178459484 | 48% |
Reaction Steps
A solution of 7-chloro-3-(ethoxycarbonyl)pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione (500 mg, 1.56 mmol), 2-propanol (60 mL), and concentrated hydrochloric acid (3 drops) was subjected to three cycles of partial solvent removal by slow distillation (over 6 hours) followed by overnight reflux. After the third cycle, solvent was removed by rotary evaporation and the crude product was purified by flash chromatography eluting with dichloromethane:2-propanol (95:5-85:15) to yield the title compound as a white solid (256 mg, 48%, m.p. 291° C.). Alternatively, the title compound can be prepared as described in Example 18 shown hereinbelow in Table 1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313290B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-f09f6840a9a2425b820a8476986ec3bd |
| Source note | uspto-grants-2001_11 |