HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23361999, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | HCID 54543367 | HCID 54543367 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 23361999 | HCID 23361999 | 80.8% |
Reaction Steps
Phosphorus pentasulphide (0.6 g, 2.5 mmol) was added to a stirred solution of 4-trifluoromethyl-9,10-dihydrodibenzo[b,f][1,4]thiazepin-11-one (0.59 g, 2 mmol) in pyridine (20 ml). The mixture was heated under reflux for 6.5 hr and then at room temperature overnight before hot water (40 ml) added. Filtration and recrystallisation from ethanol gave the title compound as fine yellow needles (0.503 g, m.p. 265°-267° C., Rf 0.65, petrol/EtOAc 1:1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05589474 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-e6a7b472946e4e53ac618a2847bf25e9 |
| Source note | uspto-grants-1996_12 |