Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethylparaben → Ethyl 4-[[1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]oxy]benzoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethylparaben | HCID 8434 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| 반응물 | 1-[3-(Trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-ol | HCID 24587632 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Ethyl 4-[[1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]oxy]benzoate | HCID 67340092 | 49% |
반응 단계
DIAD (2.262 mL, 11.49 mmol) was added to 1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-ol (3 g, 10.44 mmol), ethyl 4-hydroxybenzoate (1.909 g, 11.49 mmol) and triphenylphosphine (3.01 g, 11.49 mmol) in THF (50 mL) under nitrogen. The resulting solution was stirred at ambient temperature for 4 hours. The crude product was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 2M ammonia in methanol. The crude solid was triturated with MeOH to give a solid which was collected by filtration and dried under vacuum to give ethyl 4-[[1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]oxy]benzoate (2.220 g, 49%) as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08003649B2 |
| 출처 데이터셋 | uspto-grants-2011_08 |
| ORD ID | ord-e285951983c746dea8f975daf6143ef3 |
| 출처 메모 | uspto-grants-2011_08 |