Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,4-Dioxane → 1,4-Diazabicyclo(3.2.2)nonane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 1,4-Diazabicyclo(3.2.2)nonan-3-one | HCID 4401850 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1,4-Diazabicyclo(3.2.2)nonane | HCID 398407 | 78% |
반응 단계
To the solution of 1,4-diazabicyclo[3.2.2]nonan-3-one (15.8 g; 113 mmol) in absolute dioxane (130 ml) LiAlH4 (4.9 g; 130 mmol) was added under argon. The mixture was refluxed for 6 hours and then allowed to reach room temperature. To the reaction mixture water (5 ml in 10 ml of dioxane) was added by drops, the mixture was stirred for 0.5 hour and then filtered off via glass filter. The solvent was evaporated and the residue was distilled using Kugelrohr apparatus at 90° C. (0.1 mbar) to yield 1,4-diazabicyclo[3.2.2]nonane (11.1 g; 78%) as colourless hygroscopic material.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08372832B2 |
| 출처 데이터셋 | uspto-grants-2013_02 |
| ORD ID | ord-371ef7de77084b798bb3c052c3c1ddf7 |
| 출처 메모 | uspto-grants-2013_02 |