HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 2,7-Di-(pyrrolidinomethyleneamino)-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 1-Pyrrolidinecarboxaldehyde | HCID 77372 | — |
| Reactant | 2,7-Diamino-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene | HCID 12507062 | — |
| Reactant | Chloroform methanol | HCID 21584188 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2,7-Di-(pyrrolidinomethyleneamino)-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene | HCID 13345862 | 68% |
Reaction Steps
A suspension of 2,7-diamino-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene (500 mg) in tetrahyrofuran (4 ml) was added to a mixture of phosphorus oxychloride (0.7 ml) and N-formylpyrrolidine (2 ml) and tetrahydrofuran (4 ml), the temperature of the mixture being kept at 5° C. The resulting mixture was stirred for 30 minutes at room temperature, heated at 80° C. for 1 hour and worked up as described in Example 1, paragraph 1. Yield 68%, melting point 275° C. (decomposition) (CHCl3 /methanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04599409 |
| Source dataset | uspto-grants-1986_07 |
| ORD ID | ord-7bcbf0c91f254bc3b16ead79e10d1623 |
| Source note | uspto-grants-1986_07 |