참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Ethyl isocyanate | HCID 8022 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-(7-Chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine | HCID 90010064 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 72189950 | HCID 72189950 | 16% |
반응 단계
To a mixture of 4-(7-chloro-1,3-benzodioxol-5-yl)-2-pyrimidin-2-yl-5-(trifluoromethyl)pyrazol-3-amine (0.200 g, 0.50 mmol) and NaH (0.015 g, 0.64 mmol) in tetrahydrofurane is added ethylisocyanate (0.078 g, 1.10 mmol). The mixture is refluxed for 4 hours. The reaction was cooled to room temperature (20-25° C.), diluted with water and extracted with ethyl acetate; the organic layer separated and further washed with water and then dried and concentrated. The residue was re-crystallized with a mixture of ethyl acetate and petrole ether to give the title compound (46 mg; 16%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09174967B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-b7c683e1709b4d04807de170b618379b |
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| 출처 메모 | uspto-grants-2015_11 |
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