참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Piperazine-2,6-dione | HCID 338690 | — |
| 반응물 | 1-(3-Chloropropyl)-4-(4-fluorophenyl)piperazine | HCID 10682556 | — |
| 반응물 | 4-(2-Pyridylmethyl)-2,6-piperazinedione | HCID 14882692 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 14098744 | HCID 14098744 | 60% |
반응 단계
A suspension of 0.098 mole of sodium hydride in 30 ml of anhydrous dimethylformamide is heated to 60° C. A solution of 0.098 mole of 4-(2-pyridylmethyl)-2,6-piperazinedione in 15 ml of anhydrous dimethylformamide is added dropwise. When the addition is complete, the mixture is maintained at 60° C. for two hours. The reaction medium is then cooled to 25° C. and a solution of 0.126 mole of 4-(4-fluorophenyl)-1-(3-chloropropyl)piperazine in 10 ml of anhydrous dimethylformamide and 0.1 g of sodium iodide are added rapidly. The mixture is heated to 70° C. until the starting 2,6-piperazinedione has completely disappeared. The reaction medium is concentrated under vacuum. The solid residue is recrystallized in a mixture of iospropyl ether and ethanol (90:10). Pure crystals of 4-(2-pyridylmethyl)-1-{3-[1-(4-fluorophenyl)-4-piperazinyl]propyl}-2,6-piperazinedione are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04820707 |
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| 출처 데이터셋 | uspto-grants-1989_04 |
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| ORD ID | ord-f0211a96b6194ac891fa2adc428419f0 |
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| 출처 메모 | uspto-grants-1989_04 |
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