참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 1-Methyl-2,4,6(1H,3H,5H)-pyrimidinetrione | HCID 75722 | — |
| 생성물 | 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione | HCID 96141 | 71.6% |
반응 단계
Water (2.7 mL) is added dropwise to a suspension of 1-methylpyrimidine-2,4,6(1H,3H,5H)-trione (14.2 g, 100 mol) in POCl3 (95 mL) at 0° C. The reaction mixture is then heated at 80° C. for 5 hours. The resulting brownish solution is cooled, and POCl3 is evaporated under reduced pressure. The residue is treated with MeOH, and the obtained solid is recrystallized from ethanol to give 11.5 g product (Yield: 71.6%). m.p.=279-282° C. (dec) [Lit.2: 280-282° C.]. 1H NMR (400 MHz, DMSO-d6) δ3.10 (S, 3H), 5.90 (S, 1H), 12.4 (br, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09255099B2 |
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| 출처 데이터셋 | uspto-grants-2016_02 |
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| ORD ID | ord-8cdfce3fbab8447db49365dae93cabe6 |
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| 출처 메모 | uspto-grants-2016_02 |
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