Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Carbonate → 5-(2,2,2-Trifluoro-1,1-dimethyl-ethoxy)-pyridine-2-carbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,1,1-Trifluoro-2-methylpropan-2-ol | HCID 68182 | — |
| 반응물 | 2-Cyano-5-fluoropyridine | HCID 11332453 | — |
| 용매 | Hexamethylphosphoramide | HCID 12679 | — |
| 생성물 | 5-(2,2,2-Trifluoro-1,1-dimethyl-ethoxy)-pyridine-2-carbonitrile | HCID 57656626 | 79.4% |
반응 단계
Add 2-trifluoromethyl-2-propanol (1.1 g, 8.3 mmol) slowly to a slurry of sodium hydride (202 mg, 60% mineral oil, washed with hexane) in HMPA (3 mL) under nitrogen. Stir the slurry for 15 min, then add 5-fluoro-pyridine-2-carbonitrile (510 mg, 4.2 mmol). Stir the slurry for 16 h at ambient temperature. Adjust the mixture to pH 9 with sodium carbonate then extract with diethyl ether (3×50 mL). Collect the organic layer, dry over Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (95/5 to 80/20) to obtain the desired intermediate (768 mg, 79%). GC-MS m/z: 230 (Me).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08022062B2 |
| 출처 데이터셋 | uspto-grants-2011_09 |
| ORD ID | ord-a77b1277e1ac4efd8e56ec36ce2c3f17 |
| 출처 메모 | uspto-grants-2011_09 |