関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Benzyl-4-[4-(5-nitro-pyridin-2-yl)-piperazin-1-yl]-phthalazine | HCID 59240646 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-pyridin-3-ylamine | HCID 59240540 | 70% |
反応手順
1-Benzyl-4-[4-(5-nitro-pyridin-2-yl)-piperazin-1-yl]-phthalazine (500 mg, 1.17 mmol), iron powder (523 mg, 9.38 mmol), ammonium chloride (125 mg, 0.234 mmol), ethanol (6 mL) and water (1.5 mL) are all combined in 50 mL round bottom flask with stir bar. The mixture is stirred and heated to 70° C. for 4 h. Material is filtered through a pad of Celite and washed with CH2Cl2. Concentrate to remove all ethanol and residual water. The residue is purified by flash chromatography on silica gel (0-18% MeOH/CH2Cl2) to afford the title compound (323 mg, 70%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08536168B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-1c09af0236714b09964a6dfb6776305b |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|