Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 1-Oxa-3,8-diazaspiro(4.5)decan-2-one, 8-benzyl-
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 4-(Aminomethyl)-1-benzylpiperidin-4-ol | HCID 10421026 | — |
| 반응물 | Phosgen toluene | HCID 19083224 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-Oxa-3,8-diazaspiro(4.5)decan-2-one, 8-benzyl- | HCID 199815 | — |
반응 단계
To a solution of crude 1-benzyl-4-hydroxy-4-aminomethyl piperidine, as described above in Step A, (˜3.1 gm, 12 mmol) in acetonitrile (50 mL) containing triethyl amine (5.7 mL, 42 mmol) cooled in an ice bath was added in 1 mL portions 20% phosgene/toluene (9 mL) over a three hour period. The reaction mixture was stirred at ambient temp. for 15 hours and diluted with ethyl acetate. This solution was washed with water (2×) and the organic layer dried (anhyd. sodium sulfate), filtered, and the solvent removed under vacuum. The residue was triturated with diethyl ether and the title compound collected by filtration as a white solid, mp: 159-161° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06172076B2 |
| 출처 데이터셋 | uspto-grants-2001_01 |
| ORD ID | ord-52baa319d75b4b72b9b4abc10cab7d1f |
| 출처 메모 | uspto-grants-2001_01 |