HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 7-Chloro-3-[[(tert-butylamino)oxy]carbonyl]pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | N-tert-butylhydroxylamine hydrochloride | HCID 2777896 | — |
| Reactant | HCID 178524941 | HCID 178524941 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 7-Chloro-3-[[(tert-butylamino)oxy]carbonyl]pyrazolo[3,4-c][1]benzazepine-4,10(1H,9H)-dione | HCID 178449947 | 61% |
Reaction Steps
A solution of 7-chloro-3-(carboxy)pyrazolo[3,4-c][1]-benzazepine-4,10(1H,9H)-dione (400 mg, 1.37 mmol) (compound of Example 9) and 1,1′-carbonyldiimidazole (334 mg, 2.06 mmol) in N,N-dimethylformamide (16 mL) was stirred for 1 hour. In one portion, N-tert-butylhydroxylamine hydrochloride (516 mg, 4.11 mmol) was added and the solution was stirred for 17 hours at room temperature. To the resulting solution was added water (20 mL). The insoluble material was filtered and washed with hot methanol (3×20 mL) to give the title compound (300 mg, 61% yield, m.p. 258° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06313290B1 |
| Source dataset | uspto-grants-2001_11 |
| ORD ID | ord-51e08f90a2bb441ea101b0be1eafcb1e |
| Source note | uspto-grants-2001_11 |