Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Gamma-Butyrolactone → 1,3-Dioxo-6-hydroxy-1(3'-tert-butyl-phenyl)-hexane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Gamma-Butyrolactone | HCID 7302 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 1-(3-tert-Butylphenyl)ethan-1-one | HCID 13657978 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 1,3-Dioxo-6-hydroxy-1(3'-tert-butyl-phenyl)-hexane | HCID 57839120 | — |
반응 단계
To a stirring suspension of NaH (60% in oil, 7.66 g) in ether (480 ml) at 0° C. was added ethanol (479 μL), followed by γ-butyrolactone (6.18 ml). This was followed by dropwise addition of 1-(3-tert-butyl-phenyl)-ethanone (13.5 g) in ether (80 ml). The resulting mixture was allowed to warm to room temperature and stirred for 72 hours. After careful addition of ethanol (10.5 ml), ammonium chloride solution (10 g in 250 ml water) was then added, ether layer was then separated and washed with brine (300 ml), dried over MgSO4 and concentrated in vacuo to give 1,3-dioxo-6-hydroxy-1(3′-tert-butyl-phenyl)-hexane as crude product (18.5 g). This required no purification and was immediately used in the next reaction.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07589095B2 |
| 출처 데이터셋 | uspto-grants-2009_09 |
| ORD ID | ord-44a0741dc5894e7abf0078fe50f4a301 |
| 출처 메모 | uspto-grants-2009_09 |