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Sodium Hydroxide → 1,10-Phenanthrolin-5-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 5-Nitro-1,10-phenanthroline | HCID 72790 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1,10-Phenanthrolin-5-amine | HCID 606970 | 62% |
反応手順
A magnetically stirred solution of 5nitro-1, 10-phenanthroline (2,.01 g, 8.93 mmol) and tin(II) chloride dihydrate (6.05 g, 26.81 mmol) was heated to reflux for 3 h in ethanol (100 mL) and then concentrated in vacuo to give a viscous residue. The residue was treated with concentrated NaOH and then extracted with CHCl3 (3×50 mL). The organic layer was separated, washed with water (2×50 mL) and brine (1×50 mL), dried over anhydrous sodium sulfate, and then concentrated in vacuo to afford 1.08 g (62%) of the amine as a tan solid: m.p. 255-258 C; MS(fab):m/e 196 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05157032 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-9f4836717b7c4935b2c12884dda28557 |
| 出典メモ | uspto-grants-1992_10 |