참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dibromoethane | HCID 7839 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 5-(Benzyloxy)-2-(hydroxymethyl)-1,4-dihydropyridin-4-one | HCID 2801564 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | (2,3-Dihydro-[1,4]dioxino[2,3-c]pyridin-7-yl)methanol | HCID 21873770 | — |
반응 단계
A solution of (a) (2 g, 8.7 mmol) in water (220 ml) containing sodium hydroxide (17 mmol) was hydrogenated over 10% palladium on charcoal (1g) for 4 hours. The mixture was filtered and evaporated to give a white solid. This solid was dissolved in N,N-dimethylformamide (8 ml) then treated with potassium carbonate (2.9 g) and 1,2-dibromoethane (0.6 ml, 7 mmol). The mixture was heated at 85° C. overnight. The cooled mixture was evaporated onto silica and chromatographed eluting with 10–30% methanol in ethyl acetate affording a white solid (250 mg, 21%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07186730B2 |
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| 출처 데이터셋 | uspto-grants-2007_03 |
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| ORD ID | ord-6df80c77512540ffab3b8030403fbebe |
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| 출처 메모 | uspto-grants-2007_03 |
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