참여 물질
| 역할 | 이름 | HCID | 투입량 |
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| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 6-ethyl-5-iodo-1H-pyrimidin-4-one | HCID 178437744 | — |
| 생성물 | 4-Chloro-6-ethyl-5-iodopyrimidine | HCID 10978487 | — |
반응 단계
21.7 g (0.087 mol) of 4-hydroxy-5-iodo-6-ethylpyrimidine are stirred into 50 ml of phosphorus oxychloride which has been heated to 60° C., a slightly exothermic reaction taking place. The temperature is kept constant at 60° C. and the mixture is left for one hour to complete the reaction. The mixture is then poured onto ice-water and stirred for 30 minutes in order to hydrolyse completely the excess phosphorus oxychloride. Extraction with ethyl acetate yields 23.5 g of crystalline crude product. Recrystallisation from a mixture of 1 part ethyl acetate and 10 parts hexane yields 18.8 g (80.7% of the theoretical yield) of pure substance; m.p. 56°-57° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05468751 |
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| 출처 데이터셋 | uspto-grants-1995_11 |
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| ORD ID | ord-dc2d2da3e86a46dfb1b8ea1d9644cca0 |
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| 출처 메모 | uspto-grants-1995_11 |
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