참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 1-Benzyl-4-[4-(5-nitro-pyridin-2-yl)-piperazin-1-yl]-phthalazine | HCID 59240646 | — |
| 촉매 | Iron | HCID 23925 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6-[4-(4-Benzyl-phthalazin-1-yl)-piperazin-1-yl]-pyridin-3-ylamine | HCID 59240540 | 70% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08536168B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-1c09af0236714b09964a6dfb6776305b |
|---|
| 출처 메모 | uspto-grants-2013_09 |
|---|