Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl Acetate → 6-[4-[4-(Diphenylmethoxy)piperidino]butylamino][1,2,4]triazolo[4,3-b]pyridazine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 6-Chloro-[1,2,4]triazolo[4,3-b]pyridazine | HCID 313624 | — |
| 반응물 | 1-Piperidinebutanamine, 4-(diphenylmethoxy)- | HCID 11739259 | — |
| 용매 | 1-Butanol | HCID 263 | — |
| 생성물 | 6-[4-[4-(Diphenylmethoxy)piperidino]butylamino][1,2,4]triazolo[4,3-b]pyridazine | HCID 15524151 | 39.4% |
반응 단계
1.15 g of 4-(diphenylmethoxy)-1-piperidinebutanamine and 578 mg of 6-chloro[1,2,4]triazolo[4,3-b]pyridazine were dissolved in 20 ml of 1-butanol; 1.17 ml of N-ethyldiisopropylamine was added, followed by refluxing under heating for 14 hours. After cooling, ethyl acetate was added; the reaction mixture was washed with aqueous sodium bicarbonate and saturated saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with ethyl acetate-methanol-triethylamine (50:5:1). The desired fraction was collected and concentrated under reduced pressure; the residue was crystallized from ethyl acetate and dried to yield 611 mg of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06610694B1 |
| 출처 데이터셋 | uspto-grants-2003_08 |
| ORD ID | ord-b5bf99c2ffe947f096ecd639dfe4e842 |
| 출처 메모 | uspto-grants-2003_08 |