참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 2-(4-Morpholinyl)acetohydrazide | HCID 351635 | — |
| 반응물 | Ethyl[2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate | HCID 76754608 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | HCID 178517484 | HCID 178517484 | — |
반응 단계
1.33 g (4.7 mmol) of ethyl [2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate (Example 128A) and 740 mg (4.7 mmol) of 2-morpholin-4-ylacetohydrazide are dissolved in NMP (6 ml) and stirred in a flask with a calcium chloride drying tube at an oil-bath temperature of 160° C. for 3 h. The reaction mixture is cooled to RT and ethyl acetate (100 ml) and water (50 ml) are added. The organic phase is separated off, dried with magnesium sulphate and concentrated. The residue is chromatographed on silica gel (mobile phase dichloromethane/methanol 100:1 to 50:1). 1.25 g (70% of theory) of the product are obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09051323B2 |
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| 출처 데이터셋 | uspto-grants-2015_06 |
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| ORD ID | ord-6b0892285c6e47288621ff5cef23f71e |
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| 출처 메모 | uspto-grants-2015_06 |
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