참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| 반응물 | 3-Nitrobenzene-1-thiol | HCID 243576 | — |
| 반응물 | (2-((3-Fluorophenyl)amino)-4-(propylamino)pyrimidin-5-yl)methanol | HCID 90052116 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Tributylphosphine | HCID 13831 | — |
| 생성물 | HCID 90052119 | HCID 90052119 | 63.5% |
반응 단계
To a solution of (2-((3-fluorophenyl)amino)-4-(propylamino)pyrimidin-5-yl)methanol (E13, 20 mg) and 3-nitrothiophenol (17 mg) in tetrahydrofuran (1 mL), tributylphosphine (36 μL) and 1,1′-(azodicarbonyl)dipiperidine (28 mg) were added under ice cooling, and the mixture was stirred at room temperature for 6 hours and 30 minutes. To the reaction mixture, tributylphosphine (36 μL) and 1,1′-(azodicarbonyl)dipiperidine (28 mg) were added at room temperature, and the mixture was stirred at the same temperature for 8 hours and 30 minutes. The solvent was evaporated under reduced pressure, and then the obtained residue was purified by basic silica gel column chromatography (eluent, 88 to 40% hexane in ethyl acetate) to obtain N2-(3-fluorophenyl)-5-(((3-nitrophenyl)thio)methyl)-N4-propylpyrimidine-2,4-diamine (E19, 19 mg) as yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09145415B2 |
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| 출처 데이터셋 | uspto-grants-2015_09 |
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| ORD ID | ord-20c14a64133e4d859015f1104817bb2c |
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| 출처 메모 | uspto-grants-2015_09 |
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