Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethylene Glycol → 3-Hydroxy-5beta-estran-17-one ethylene ketal
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethylene Glycol | HCID 174 | — |
| 반응물 | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| 반응물 | Ethyl acetate hexane | HCID 21226206 | — |
| 반응물 | 3-Hydroxy-5betaestran-17-one | HCID 22795659 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-Hydroxy-5beta-estran-17-one ethylene ketal | HCID 86760179 | 94.8% |
반응 단계
Compound 4(10 g, 36.2 mmol) was dissolved in dry benzene (150 ml) mixed with ethylene glycol (25 ml, 280 mmol) and pyridinium p-toluenesulfonate (1 g, 3.9 mmol) and refluxed using a Dean-stark separator overnight till no starting material was detected by TLC. The cold solution was diluted with EtOAc (100 ml), washed twice with brine, dried on Na2SO4 and the solvents removed under reduced pressure. Flash-chromatography on silica gel with EtOAc: Hexane 4:6 as eluant to give 11.0 g (94.5% yield) the title compound as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07087590B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-faa2f348d6f5478eb5c5bd468fd5e72f |
| 출처 메모 | uspto-grants-2006_08 |