Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Bicarbonate → Ethanone, 1-[6-(2,2,2-trifluoroethoxy)-3-pyridinyl]-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | N-methoxy-N-methyl-6-(2,2,2-trifluoroethoxy)pyridine-3-carboxamide | HCID 86707284 | — |
| 반응물 | HCID 178418573 | HCID 178418573 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Ethanone, 1-[6-(2,2,2-trifluoroethoxy)-3-pyridinyl]- | HCID 58629124 | 83% |
반응 단계
To a stirred solution of N-methoxy-N-methyl-6-(2,2,2-trifluoroethoxy)nicotinamide (6.54 g, 24.8 mmol, Step-2) in tetrahydrofuran (80 mL) is added dropwise 1.06M methylmagnesium bromide (46.7 mL, 49.5 mmol) at 0° C. The reaction mixture is stirred at room temperature for 1.5 hours. The reaction mixture is poured into saturated aqueous sodium hydrogen carbonate (100 mL) and extracted with ethyl acetate (300 mL). The organic layer is washed with water (100 mL×2) and dried over sodium sulfate and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (1:1) to give 4.51 g (83% yield) of the title compound as colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09302991B2 |
| 출처 데이터셋 | uspto-grants-2016_04 |
| ORD ID | ord-022f4767b1264c60b3aa5b35c2f153ea |
| 출처 메모 | uspto-grants-2016_04 |