Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Toluene → N'-[3-tert-butyl-1-[[(5R)-5-methyloxolan-2-yl]methyl]pyrazol-5-yl]-N,N-dimethylmethanimidamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | HCID 178484244 | HCID 178484244 | — |
| 촉매 | Tetraethylammonium Iodide | HCID 6225 | — |
| 촉매 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 촉매 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 생성물 | N'-[3-tert-butyl-1-[[(5R)-5-methyloxolan-2-yl]methyl]pyrazol-5-yl]-N,N-dimethylmethanimidamide | HCID 87439811 | 25% |
반응 단계
To a solution of Example 63A (1.6 g, 8.2 mmol) in toluene (100 mL) were added potassium carbonate (2.3 g, 16.5 mmol), Example 64B (2.7 g, 9.9 mmol), tetrabutylammonium iodide (70 mg), tetraethylammonium iodide (70 mg) and tetrabutylammonium hydrogensulfate (70 mg). The reaction mixture was refluxed for 16 h, cooled, filtered and concentrated under reduced pressure. The residue was purified by column chromatography using an Analogix® Intelliflash280 T (SiO2, 0-10% methanol in dichloromethane) to provide 0.6 g (25%) of the title compound. MS (ESI+) m/z 293 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09193713B2 |
| 출처 데이터셋 | uspto-grants-2015_11 |
| ORD ID | ord-94790b9ad81e42a0b6f73d231cea1879 |
| 출처 메모 | uspto-grants-2015_11 |