참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-(5-Isoquinolinylsulfonyl)piperazine | HCID 3545 | — |
| 반응물 | Benzyl Chloride | HCID 7503 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 13116945 | HCID 13116945 | 79% |
반응 단계
In 150 ml of ethanol were added 2.77 g of 1-(5-isoquinolinesulfonyl)piperazine, i.e., Compound (35), 1.0 g of potassium hydroxide and 1.9 g of benzyl chloride, and the mixture was refluxed under heating for five hours. After the ethanol was removed from the reaction solution, 100 ml of chloroform was added to the resulting solution, and the solution obtained was washed with a buffer solution having a pH of 5.5 and extracted twice with 20 ml of a 2N aqueous hydrochloric acid solution. The aqueous hydrochloric acid layer was rendered alkaline, extracted twice with 50 ml of chloroform, and the chloroform layer extracted was washed with water and dried with anhydrous magnesium sulfate. After the chloroform was distilled therefrom under reduced pressure, 5 ml of a 10N aqueous hydrochloric acid solution was added to the residue and the mixture was condensed to dryness. The crystalline residue thus obtained was recrystallized from ethanol to give 2.9 g of 1-(5-isoquinolinesulfonyl)-4-benzylpiperazine [i.e., Compound (56)] dihydrochloride in a yield of 66%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04525589 |
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| 출처 데이터셋 | uspto-grants-1985_06 |
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| ORD ID | ord-58ea52aa69d445779864ee86e92909c3 |
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| 출처 메모 | uspto-grants-1985_06 |
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