Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
5-[2-(3-Ethylphenyl)ethyl]-2-methyloxazole-4-carboxylic acid → 7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 5-[2-(3-Ethylphenyl)ethyl]-2-methyloxazole-4-carboxylic acid | HCID 22003640 | — |
| 용매 | Thionyl Chloride | HCID 24386 | — |
| 생성물 | 7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-one | HCID 22003584 | — |
반응 단계
A solution of the product from step (vii) (9.5 g) in thionyl chloride (100 ml) was stirred at room temperature for 4 days. After removal of solvent under reduced pressure, the residue was dissolved in 1,2-dichloroethane (200 ml) and treated with aluminium chloride (23 g). The reaction mixture was heated at reflux for 1 hour and allowed to cool. The resultant suspension was partitioned between 10% hydrochloric acid and dichloromethane. The combined extracts were evaporated, triturated with acetonitrile, and filtered through a plug of celite. Evaporation afforded a residue which was purified by chromatography eluting with 50-100% ethyl acetate in isohexane.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06218376B1 |
| 출처 데이터셋 | uspto-grants-2001_04 |
| ORD ID | ord-439642bca3914b95b6b9a3dedface89f |
| 출처 메모 | uspto-grants-2001_04 |