Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Methylcyclopentene → 5-Methyl-6-azabicyclo[3.2.0]heptan-7-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Methylcyclopentene | HCID 12746 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Sodium Sulfite | HCID 24437 | — |
| 반응물 | Chlorosulfonyl isocyanate | HCID 70918 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 5-Methyl-6-azabicyclo[3.2.0]heptan-7-one | HCID 10772975 | — |
반응 단계
To a solution of 1-methylcyclopent-1-ene (CAS number 693-89-0; 38.5 mL, 365 mmol) in diethyl ether (220 ml) at 0° C. was added drop wise [(chlorosulfonyl)imino]methanone (CAS number 1189-71-5; 33.3 ml, 383 mmol). The reaction was then allowed to warm to room temperature and then heated to 36° C. for 72 hours. The reaction was then cooled to room temperature and a solution of sodium sulfite (73.5 g) in water (400 ml) was added drop wise, followed by the addition of 15% w/v potassium hydroxide (500 ml) to obtain pH 7-8. The phases were separated and aqueous phase was extracted with diethyl ether (2×200 ml). The combined organics were dried over magnesium sulfate and concentrated in vacuo to afford the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09156829B2 |
| 출처 데이터셋 | uspto-grants-2015_10 |
| ORD ID | ord-5e70b3aa1f97443bbde24760afcb2e01 |
| 출처 메모 | uspto-grants-2015_10 |