Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium bis(trimethylsilyl)amide → HCID 178489756, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| 반응물 | Tert-butyl 5-amino-3-[2-(3,5-dimethoxyphenyl)ethyl]pyrazole-1-carboxylate | HCID 57440371 | — |
| 반응물 | Methyl 4-[(4-fluoropiperidin-1-yl)methyl]benzoate | HCID 57440372 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178489756 | HCID 178489756 | 16.4% |
반응 단계
A solution of NaHMDS in THF (1 M, 0.65 ml, 0.65 mmol, 1.5 eq) was added dropwise at ambient temperature to a mixture of tert-butyl 5-amino-3-[2-(3,5-dimethoxyphenyl) ethyl]pyrazole-1-carboxylate (150 mg, 0.43 mmol, 1 eq) and methyl 4-[(4-fluoropiperidin-1-yl)methyl]benzoate (131 mg, 0.52 mmol, 1.2 eq) in THF (0.5 ml). The reaction mixture was stirred at ambient temperature for 1 h. It was then concentrated and the crude product was purified by reverse-phase prep. HPLC (basic) using a 39-49% gradient of acetonitrile in water containing 1% ammonium hydroxide solution. The clean fractions were taken and evaporated to afford the title compound as a colourless solid (33 mg, 16% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07737149B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-c8a8231a872143a3b61477dd1159ada3 |
| 출처 메모 | uspto-grants-2010_06 |