Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Trifluoroacetic acid → 3-Methyl-3,9-diazaspiro[5.5]undecane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Trifluoroacetic acid | HCID 6422 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | HCID 58808179 | HCID 58808179 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Methyl-3,9-diazaspiro[5.5]undecane | HCID 21813293 | 78.5% |
반응 단계
9-Methyl-3,9-diaza-spiro[5.5]undecane-3-carboxylic acid tert-butyl ester (435 mg, 1.62 mmol) was dissolved in dichloromethane (11 mL) and cooled on ice. Trifluoroacetic acid (4 mL) in dichloromethane (5 mL) was added and the reaction mixture was stirred at room temperature for 2 h. Evaporation to dryness, co-evaporation with toluene, ethyl acetate and diethyl ether gave a foam which was dissolved in dichloromethane, and sodium hydroxide (2 N) was added. The aqueous phase was extracted five times with dichloromethane. The combined organic phase was washed with brine, dried (sodium sulfate), filtered and evaporated to give 214 mg (78%) of 3-methyl-3,9-diaza-spiro[5.5]undecane.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07943630B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-34833a95099246088d70e08d92898144 |
| 출처 메모 | uspto-grants-2011_05 |