참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Formate | HCID 2735122 | — |
| 반응물 | N-(4-Methyl-3-nitro-phenyl)-4-(4-methyl-piperazin-1-ylmethyl)-benzamide | HCID 29984087 | — |
| 촉매 | Platinum | HCID 23939 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | N-(4-Methyl-3-aminophenyl)-4-(4-methylpiperazinomethyl)benzamide | HCID 11702833 | — |
반응 단계
Alternatively a solution of N-(4-methyl-3-nitro-phenyl)-4-(4-methyl-piperazin-1-ylmethyl)-benzamide (60 g, 163 mmol) in ethanol 90% (300 ml) at room temperature under an atmosphere of nitrogen is treated sequentially with platinum (5%) on carbon (6.0 g) and potassium formate (68.5 g, 814 mmol). The resulting suspension is then heated at 80° C. for a period of 16 hrs. The reaction mixture is filtrated at 70° C. over a pad of Celite. Ethanol 90% (150 ml) and water (150 ml) are used to rinse the reactor. Ethanol is removed from the combined filtrates by distillation in vacuo at an external temperature 60° C. The crude product separates from the aqueous concentrate as an oil during the distillation, crystallizes upon subsequent cooling to 23° C. within 2 hrs and is filtered of with suction, washed with ethanol (200 ml) and dried in vacuo. Yield: 55 g of the title compound, 99% of theory, as yellowish crystals. (HPLC: 98.0% area).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07456283B2 |
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| 출처 데이터셋 | uspto-grants-2008_11 |
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| ORD ID | ord-097c97463e484d00b4cc6c6e7f9b5a62 |
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| 출처 메모 | uspto-grants-2008_11 |
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