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Phosphorus oxychloride → 3,8-Di-(pyrrolidinomethyleneamino)-6(5H)-phenanthridone
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 | 3,8-Diamino-5H-phenanthridin-6-one | HCID 283716 | — |
| 反応物 | Chloroform methanol | HCID 21584188 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3,8-Di-(pyrrolidinomethyleneamino)-6(5H)-phenanthridone | HCID 13345873 | 52% |
反応手順
A suspension of 3,8-diamino-6-(5H)-phenanthridone (500 mg) in tetrahydrofuran (5 ml) was added to a mixture of phosphorus oxychloride (0.75 ml) and N-formylpyrrolidine (2.5 ml) and tetrahydrofuran (5 ml), the temperature of the mixture being kept at 5° C. The resulting mixture was stirred for 30 minutes at room temperature, heated at 50° C. for 1 hour and worked as described in Example 8, paragraph 1. Yield 52%, melting point 280° 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-72abbf7032ed4faa95680a74f33b4c58 |
| 出典メモ | uspto-grants-1986_07 |