참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,1-Bis(2,2-dimethylpropoxy)-N,N-dimethylmethanamine | HCID 78623 | — |
| 반응물 | 5-Chloro-2(1H)-pyrimidinone | HCID 108578 | — |
| 반응물 | 5-Methylfurfuryl alcohol | HCID 520911 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 20491764 | HCID 20491764 | 22.9% |
반응 단계
N,N-Dimethylformamide dineopentyl acetal (1.8 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (522 mg) and 2-hydroxymethyl-5-methylfuran (628 mg) in dry N,N-dimethylformamide (10 ml) under nitrogen. The resulting solution was then stirred and heated at 90° C. under nitrogen. After 1.5 h the reaction mixture was evaporated to a brown crystalline solid (1.030 g). The solid was subjected to column chromatography on silica (70-230 mesh) (100 g) developing with chloroform-ethanol, 29:1. The resulting pale yellow solid (327 mg) was crystallised twice from acetone to give white needles of the title furan (206 mg), m.p. 166°-167° C., λmax 226 nm (ε 15,660), 332 nm (ε 2,520), λinf 247 nm (ε 3,100).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04399140 |
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| 출처 데이터셋 | uspto-grants-1983_08 |
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| ORD ID | ord-3c111c8bccee427da371b6fea9153b0e |
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| 출처 메모 | uspto-grants-1983_08 |
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