HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus pentachloride → HCID 86680253, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | 16367-99-0 | HCID 135431964 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 86680253 | HCID 86680253 | — |
Reaction Steps
A mixture of 23.5 g (100 mmol) of benzimidazo[1,2-c]quinazolin-6(5H)-one [16367-99-0], 22.9 g (110 mmol) of phosphorus pentachloride and 250 ml of phosphoryl chloride is heated under reflux for 24 h. The excess phosphoryl chloride is removed in vacuo, 1000 ml of dichloromethane are added to the residue, the mixture is hydrolysed by addition of 1000 g of ice, rendered weakly alkaline by addition of 10% by weight sodium hydroxide solution, the organic phase is separated off, dried over sodium sulfate, and the dichloromethane is then removed in vacuo. Yield: 24.1 g (94 mmol), 94%. Purity: >95% according to 1H-NMR.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273080B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-5dc7695b89ca4aacac4cee5972edd70c |
| Source note | uspto-grants-2016_03 |