참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Methyl-5-Nitroaniline | HCID 7444 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 4,6-Dichloropyrimidine | HCID 70943 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-[(6-Chloro)pyrimidin-4-ylamino]-1-methyl-4-nitrobenzene | HCID 86061071 | 78.6% |
반응 단계
2.64 g of 2-methyl-5-nitroaniline and 10.33 g of 4,6-dichloropyrimidine were stirred with heating at 110° C. for 16 hours. After air cooling, the reaction solution was dissolved in methanol. An aqueous saturated sodium hydrogen carbonate solution and ethyl acetate were added to separate the aqueous layer. The aqueous layer was further subjected to extraction with ethyl acetate twice. The organic layers were combined and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain a crude product. The crude product was washed with diisopropyl ether to obtain 3.61 g of the objective compound as yellow crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07728131B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-64102c395d4244efb41b9d6bfcb88a88 |
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| 출처 메모 | uspto-grants-2010_06 |
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