Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Lithium Hydroxide → 4-(4-(Tert-butoxycarbonyl)piperazin-1-yl)-3-fluorobenzoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Lithium Hydroxide | HCID 3939 | — |
| 반응물 | Tert-butyl 4-(2-fluoro-4-(methoxycarbonyl)phenyl)piperazine-1-carboxylate | HCID 23117202 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 4-(4-(Tert-butoxycarbonyl)piperazin-1-yl)-3-fluorobenzoic acid | HCID 59416800 | 100% |
반응 단계
tert-butyl 4-(2-fluoro-4-(methoxycarbonyl)phenyl)piperazine-1-carboxylate 301 (4.6 g, 13.59 mmol) was suspended in 1,4-dioxane (68.0 mL) and treated with 1N LiOH (68.0 mL, 68.0 mmol). The reaction mixture was stirred at room temperature for 23 h. The reaction mixture was concentrated in vacuo until most of the dioxane was gone and acidified with HCl (4.5 N) until a thick precipitate resulted. The precipitate was filtered, washed with water, and dried in vacuum to afford the title compound as a brown solid (4.40 g, 13.57 mmol, 100% yield). ESI-MS: m/z 325 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08669249B2 |
| 출처 데이터셋 | uspto-grants-2014_03 |
| ORD ID | ord-d70a773b14cd436eb3643879360a0ead |
| 출처 메모 | uspto-grants-2014_03 |