참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | Methyl 2,6-dichloro-5-methoxypyrimidine-4-carboxylate | HCID 11514203 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Methyl 6-amino-2-chloro-5-methoxypyrimidine-4-carboxylate | HCID 52270701 | 50% |
반응 단계
A solution comprising the reaction mixture prepared by Example 8, which reaction mixture contained the methyl 2,6-dichloro-5-methoxy-pyrimidine-4-carboxylate (25 g, 0.1 mol), and dimethyl sulfoxide (DMSO) was prepared. To this solution was added, at 0-5° C., a solution of ammonia in DMSO (2 eq). This mixture was stirred at the same 0-5° C. temperature for 10 to 15 minutes. Later, the mixture was diluted with ethyl acetate, and the resulting solid was filtered. The filtrate was washed with a brine solution. The organic layer was dried over sodium sulfate. Upon concentration, the crude product was obtained. The crude product was stirred in a minimum amount of ethyl acetate and filtered to obtain the pure compound. The resulting filtrate, after concentration, was column purified. This produced the title compound (11 g, 50% yield): mp 158° C.; 1H NMR (DMSO-d6) δ 3.71 (s, 3H), 3.86 (s, 3H), 7.65 (brs, 1H), 8.01 (brs, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09216958B2 |
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| 출처 데이터셋 | uspto-grants-2015_12 |
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| ORD ID | ord-51840dbd9e4f480782764f0cae77de02 |
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| 출처 메모 | uspto-grants-2015_12 |
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