Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 1-(4-{[tert-Butyl(dimethyl)silyl]oxy}cyclohexyl)-3-(trifluoromethyl)-1H-pyrazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 3-(Trifluoromethyl)pyrazole | HCID 1807034 | — |
| 반응물 | 4-{[tert-Butyl(dimethyl)silyl]oxy}cyclohexyl methanesulfonate | HCID 86634656 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(4-{[tert-Butyl(dimethyl)silyl]oxy}cyclohexyl)-3-(trifluoromethyl)-1H-pyrazole | HCID 59556059 | 44% |
반응 단계
To a solution of 3-trifluoromethyl-1H-pyrazole (1.0 g, 7.35 mmol) in DMF (10 mL) cooled in an ice bath was added NaH (0.3 g, 60% in mineral oil). The mixture was stirred for 10 minutes before the mesylate (1.13 g, 3.68 mmol) of step B in DMF (5 mL) was added. Stirring was continued at room temperature for 1 hour and then at 100° C. overnight. After being cooled to room temperature, the solution was poured into ice water and extracted with EtOAc three times. The combined extract was washed with brine, dried over MgSO4 and concentrated. Purification on silica gel eluting with 5:1 EtOAc/hexanes provided the title compound (0.56 g, 44%) as an oil. MS calculated (M+H)+ 349. found 349.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07985730B2 |
| 출처 데이터셋 | uspto-grants-2011_07 |
| ORD ID | ord-162b2bc945a0480491a8f55a45f6a173 |
| 출처 메모 | uspto-grants-2011_07 |