참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | HCID 178494688 | HCID 178494688 | — |
| 용매 | 1,1-Dichloroethane | HCID 6365 | — |
| 생성물 | 4-Chloro-5-methoxy-6-(methoxymethyl)pyrimidine | HCID 15279350 | — |
반응 단계
85.0 g (0.5 mol) of 4-hydroxy-5-methoxy-6-methoxymethylpyrimidine were suspended in 600 ml of dichloroethane, 50.5 g of triethylamine were added, and 260 g (1.7 mol) of phosphorus oxychloride were then added without cooling. The mixture was stirred for 3 hours at 80° C., poured into ice-water and neutralized by adding solid sodium carbonate, the organic phase was separated, and the water phase was extracted several times by stirring with methylene chloride. The combined organic phases were dried and concentrated. The residue was distilled under a water pump vacuum. 66.1 g (70% of theory) of a yellow oil were obtained. B.p. 93°-96° C./0.1mm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05668140 |
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| 출처 데이터셋 | uspto-grants-1997_09 |
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| ORD ID | ord-3d4eae15b48d410c83b87577a98525b3 |
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| 출처 메모 | uspto-grants-1997_09 |
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