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Phosphorus oxychloride → 2,7-Di-(pyrrolidinomethyleneamino)-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 1-Pyrrolidinecarboxaldehyde | HCID 77372 | — |
| 反応物 | 2,7-Diamino-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene | HCID 12507062 | — |
| 反応物 | Chloroform methanol | HCID 21584188 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2,7-Di-(pyrrolidinomethyleneamino)-5,10-dioxo-4,5,9,10-tetrahydro-4,9-dioxapyrene | HCID 13345862 | 68% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04599409 |
| 出典データセット | uspto-grants-1986_07 |
| ORD ID | ord-7bcbf0c91f254bc3b16ead79e10d1623 |
| 出典メモ | uspto-grants-1986_07 |