Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 5-fluoro-1-(2-fluoro-phenyl)-3-(1-methyl-piperidin-3-ylmethoxy)-1H-indazole hydrogen chloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3-[5-fluoro-1-(2-fluoro-phenyl)-1H-indazol-3-yloxymethyl]-3-methyl-piperidine-1-carboxylic acid tert-butyl ester | HCID 68531441 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 5-fluoro-1-(2-fluoro-phenyl)-3-(1-methyl-piperidin-3-ylmethoxy)-1H-indazole hydrogen chloride | HCID 68528052 | 81.7% |
반응 단계
To a room temperature stirred solution of Intermediate 57 (0.127 g, 0.278 mmol) in EtOAc (0.925 ml) was added 0.902 ml of a 4.0 M HCl solution in dioxane. The reaction was allowed to stir overnight at room temperature. Upon completion as indicated by HPLC, the reaction was concentrated under reduced pressure. EtOAc was added to the solid and then concentrated down under reduced pressure. This process was repeated five times. The solid was triturated with EtOAc/Et2O (2:1), the solid was filtered and then washed with Et2O (2×15 ml). The solid was placed in a drying oven under reduced pressure to yield 0.089 g (81.7%) of the title product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07423054B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-4d3942872b814869a0990daf77a1908c |
| 출처 메모 | uspto-grants-2008_09 |