참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Chloro-5-(chloromethyl)pyridine | HCID 155479 | — |
| 반응물 | 4-(methylamino)furan-2(5H)-one | HCID 12213511 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | 4-[[(6-chloropyridin-3-yl)methyl](methyl)amino]furan-2(5H)-one | HCID 11550459 | 87% |
반응 단계
30 g of 4-(methylamino)furan-2(5H)-one (Example 11) are initially charged in 450 ml of dimethoxyethane at room temperature. Subsequently, 12.6 g of sodium hydroxide are added and, at 40° C., 225 g of a 20% solution of 2-chloro-5-(chloromethyl)pyridine in dimethoxyethane are metered in. The mixture is stirred at 50° C. for a further 6 h. The solvent is substantially removed under reduced pressure and the residue is admixed with 300 ml of water. The solids are filtered off, washed with 150 ml of water and dried under reduced pressure. 58.7 g of 4-([[6-chloropyridin-3-yl]methyl](methy)amino)furan-2(5H)-one are obtained with a purity of 94% (this corresponds to 87% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08487112B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-8236c195a16443edb1720bb9f06d759e |
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| 출처 메모 | uspto-grants-2013_07 |
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