참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbamimidic acid, methyl ester, sulfate (1:1) | HCID 169039 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | HCID 54038767 | HCID 54038767 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178498444 | HCID 178498444 | 35.2% |
반응 단계
A mixture of methyl 2-{(3,4-difluorophenyl) methylene}-3-oxobutyrate (8.8 .g, 36.6 mmol), O-methylisourea hydrogen sulfate (9.4 g, 55 mmol), and NaHCO3 (12.3 g, 0.146 mol) in DMF (30 mL) was stirred and heated at 70° C. for 16 hours. The mixture was cooled, diluted with EtOAc (300 mL) and washed with water (5×300 mL), brine (300 mL), and dried (MgSO4). Solvent was evaporated and the crude product was purified by flash column chromatography on silica gel using 10% through 20% EtOAc in hexane as the gradient eluent, to leave the product as an oil (3.82 g, 30.2%)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06172066B2 |
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| 출처 데이터셋 | uspto-grants-2001_01 |
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| ORD ID | ord-2b9f5b52af624c5e88d7c5cb83a00e22 |
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| 출처 메모 | uspto-grants-2001_01 |
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