참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Gamma-Butyrolactone | HCID 7302 | — |
| 반응물 | Sodium hexamethyidisilazane | HCID 45051731 | — |
| 반응물 | HCID 178507322 | HCID 178507322 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178520695 | HCID 178520695 | 59% |
반응 단계
30 mg (0.068 mmol) of 1-{3-[4-(2-aminopyridin-4-yl)-1H-pyrazol-3-yl]phenyl}-3-[4-(trifluoromethyl)phenyl]urea were dissolved in 2 ml of dry tetrahydrofuran and 15 μl (0.34 mmol) of γ-butyrolactone were added. The reaction mixture was cooled to 0° C. and a solution of 680 μl (0.68 mmol) of hexamethyldisilazane sodium salt 1M in THF in 2 ml of the same solvent were added dropwise. The mixture was maintained at 0° C. for 6 hours and at room temperature overnight, then partitioned between dichloromethane and water. The organic phase was dried over sodium sulphate and evaporated. The crude was finally purified by preparative HPLC in reverse phase conditions (basic eluant), giving 20 mg (59%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541575B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-3cff4afe910941b08835c59a82d566ad |
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| 출처 메모 | uspto-grants-2013_09 |
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