Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
m-Chloroperbenzoic acid → N-[4-Cyano-3-(trifluoromethyl)phenyl]-2-methyloxirane-2-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 반응물 | N-[4-Cyano-3-(trifluoromethyl)phenyl]-2-methylprop-2-enamide | HCID 11149469 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-[4-Cyano-3-(trifluoromethyl)phenyl]-2-methyloxirane-2-carboxamide | HCID 10149314 | — |
반응 단계
460 mg of the amide (7) from the Example 1 was dissolved in 30 ml of dichloromethane. 560 mg of m-chloroperbenzoic acid (purity 70–75%) was added. The reaction mixture was stirred overnight at reflux. The reaction was monitored with HPLC. The reaction mixture was washed successively with 2×20 ml of a sodium sulfite solution, 2×20 ml of saturated aqueous NaHCO3 and 20 ml of brine. The organic layer was dried (Na2SO4), filtrated and evaporated under reduced pressure yielding the epoxide (5A) as yellow solid material. Isolated yield: 400 mg (82%). 1H- and 13C-NMR confirmed the expected structure. HPLC: 96% purity.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07186854B2 |
| 출처 데이터셋 | uspto-grants-2007_03 |
| ORD ID | ord-21cdb9439eeb4a488357142f6552a73b |
| 출처 메모 | uspto-grants-2007_03 |