HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 1-Phthalazinamine, N-(2,2-dimethylpropyl)-4-phenyl-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Neopentylamine | HCID 79882 | — |
| Reactant | 4-Phenyl-1-(2H)-phthalazinone | HCID 219150 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | P-Xylene | HCID 7809 | — |
| Product | 1-Phthalazinamine, N-(2,2-dimethylpropyl)-4-phenyl- | HCID 6410595 | — |
Reaction Steps
To a suspension of 100 g of 4-phenyl-1(2H)-phthalazinone and 96.2 g of neopentylamine in 300 ml of p-xylene were added dropwise 83.7 g of phosphorus oxychloride with stirring and the resulting mixture was stirred under reflux for 4 hours. After allowing to be cooled, a saturated aqueous solution of NaHCO3 was added to the reaction mixture. Then, the mixture was extracted with chloroform and the organic layer was separated, dried and then concentrated. The residue was recrystallized from ethanol to afford the title compound as a pale yellow crystal. 100.8 g (Yield, 77%) Melting point: 215.5°-216.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04668677 |
| Source dataset | uspto-grants-1987_05 |
| ORD ID | ord-52cf5b48f4ad4bf8a41bf72352e89312 |
| Source note | uspto-grants-1987_05 |