Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 3-Ethyl 5-methyl 6-(difluoromethyl)-4-fluoro-2-(trifluoromethyl)-3,5-pyridinedicarboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | 3-Ethyl 5-methyl 6-(difluoromethyl)-4-chloro-2-(trifluoromethyl)-3,5-pyridinedicarboxylate | HCID 14013771 | — |
| 촉매 | 18-Crown-6 | HCID 28557 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-Ethyl 5-methyl 6-(difluoromethyl)-4-fluoro-2-(trifluoromethyl)-3,5-pyridinedicarboxylate | HCID 14013772 | 97.8% |
반응 단계
The reagent was prepared by dissolving 0.37 g (0.001 mol) of 18-crown-6 in 30 ml of dry CH3CN (distilled over CaH2) and then adding 3.25 g (0.056 mol) of dry KF (dried in an oven at 50° C./67 Pa). After the heterogeneous system was mechanically stirred for 30 minutes, 10 g (0.028 mol) of product of Example 103 was added and the resulting mixture was refluxed for 6 days. The reaction mixture was poured into H2O, extracted with diethyl ether (2X), dried (MgSO4) and solvent removed in acuo affording 9.45 g of a brown oil. The crude product was purified by HPLC using 1ethyl acetate/cyclohexane as eluting solvent affording 6.72 g (70) of product as a white solid; mp 40-41° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04698093 |
| 출처 데이터셋 | uspto-grants-1987_10 |
| ORD ID | ord-bb9a5bd0d1a44d6a956d8934971a28a9 |
| 출처 메모 | uspto-grants-1987_10 |