Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 2,9-Diazaspiro(5.5)undecan-1-one hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | tert-Butyl 1-oxo-2,9-diazaspiro[5.5]undecane-9-carboxylate | HCID 49760149 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2,9-Diazaspiro(5.5)undecan-1-one hydrochloride | HCID 45074288 | 96% |
반응 단계
To the stirred solution of tert-butyl 1-oxo-2,9-diazaspiro[5.5]undecane-9-carboxylate (3.0 g, 11.19 mmol) in DCM (60 mL) was added 4N HCl in dioxane (20 mL) and the mixture was stirred at rt for 18 h. The solvent was removed under reduced pressure and triturated with diethyl ether (2×5 mL) to yield the title compound as a solid (2.2 g, 96%). Note: The product is moisture sensitive. [1H-NMR (DMSO-d6, 300 MHz): δ 9.25-8.68 (m, 2H), 7.43 (s, 1H), 7.20-6.25 (m, 2H), 3.61-2.90 (m, 5H), 2.12-1.95 (m, 2H), 1.76-1.49 (m, 5H); LCMS RtA=0.326, [M+H]+=169.0].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08530648B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-67defb743249464596a605a19e4e499a |
| 출처 메모 | uspto-grants-2013_09 |