Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
(Trifluoromethyl)trimethylsilane → 6-[2-(4-Bromo-2-chloro-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-3-methyl-3H-benzooxazol-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | (Trifluoromethyl)trimethylsilane | HCID 552549 | — |
| 반응물 | Tetrabutylammonium Fluoride Trihydrate | HCID 11726816 | — |
| 반응물 | 6-[2-(4-Bromo-2-chloro-phenyl)-propionyl]-3-methyl-3H-benzooxazol-2-one | HCID 66697107 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-[2-(4-Bromo-2-chloro-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-3-methyl-3H-benzooxazol-2-one | HCID 66697011 | — |
반응 단계
Trifluoromethyltrimethylsilane (2M in THF, 1.48 mL) was added at 0° C. to a solution of 6-[2-(4-bromo-2-chloro-phenyl)-propionyl]-3-methyl-3H-benzooxazol-2-one (531 mg) in THF (15 mL) followed by the addition of tetrabutylammonium fluoride trihydrate (424 mg). Stirring was continued for 48 hours at r.t. The reaction mixture was poured into ice/water and extracted two times with ethyl acetate. The combined organic layers were washed with brine, dried over Na2SO4, filtered and the solvent was evaporated. The residue was purified by flash chromatography (silica gel, heptane:ethyl acetate=7:3) to give the title compound as a orange amorphous foam (440 mg, 70%). MS (neg. ion, m/e)=464.0 [(M−H)−].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08450313B2 |
| 출처 데이터셋 | uspto-grants-2013_05 |
| ORD ID | ord-cc7d8695385e43a8ab60d5a58d207400 |
| 출처 메모 | uspto-grants-2013_05 |