참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Ethyl 1-benzyl-4-oxopiperidine-3-carboxylate hydrochloride | HCID 102623 | — |
| 반응물 | Formamidine acetate | HCID 160693 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Sodium Hydroxide | HCID 14798 | — |
| 생성물 | 6-benzyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidin-4(3H)-one | HCID 135592935 | — |
반응 단계
A mixture of ethyl 1-benzyl-4-oxopiperidine-3-carboxylate hydrochloride (50.0 g, 0.168 mol), formamidine acetate (16.2 g, 0.201 mol), 4.37 M of sodium methoxide in methanol (190 mL) and methanol (200 mL, 5 mol) was heated to 85° C. for 16 hour in a 350 ml sealed reaction vessel. The mixture was allowed to cool and reduced in vacuo. The residue was dissolved in 1N NaOH (150 ml) and poured over ice. Glacial acetic acid was added to the mixture until the pH of the mixture was 7 and a tan solid precipitated out. the solid was filtered, washed with water and cold ether, and dried on high vacuum to yield the title compound as a tan solid. (26.2 g, 61.4%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07745451B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-ef5a0690710f4457bbda238862f33705 |
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| 출처 메모 | uspto-grants-2010_06 |
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