HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 11820387, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 1-Methyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione | HCID 3562387 | — |
| Product | HCID 11820387 | HCID 11820387 | — |
Reaction Steps
The title compound 467 (1.54 g, 8.10 mmol) was heated in phosphorus oxychloride (15 mL) at 95° C. for 2 hours. The reaction mixture was then cooled to room temperature and excess of phosphorus oxychloride was removed under reduced pressure. The black oil was dissolved in ethyl acetate and the organic phase was washed with sodium bicarbonate (saturated solution) and brine, dried over sodium sulfate, filtered and concentrated to afford crude title compound 468 that was used as such for the next step. MS (ESI): 209.12 (MH)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09193749B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-00498f7125bb4c3fb25e41046bac7fb5 |
| Source note | uspto-grants-2015_11 |