Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hexane → Ethyl 5-Hydroxy-4-methyl-7-(1-methyl-4-phenylbutyl)coumarin-3-propionate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hexane | HCID 8058 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | Diethyl 2-acetylglutarate | HCID 73915 | — |
| 반응물 | 5-(5-Phenylpentan-2-yl)benzene-1,3-diol | HCID 20487367 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | Ethyl 5-Hydroxy-4-methyl-7-(1-methyl-4-phenylbutyl)coumarin-3-propionate | HCID 53719146 | — |
반응 단계
A mixture of 2-(3,5-dihydroxyphenyl)-5-phenylpentane (33 g., 0.13 M), (Preparation C) diethyl α-acetoglutarate (32.2 g., 0.14 M) and phosphorous oxychloride (20 g., 0.13 M), protected from atmospheric moisture, is stirred at room temperature. After 10 days, the mixture is dissolved in chloroform, washed three times with water, dried (Na2SO4), and evaporated. The residue is subjected to silica gel chromatography (eluents--9 benzene:1 ether) to yield 22 g. of the desired ester, m.p. 58°-70° C. from hexane. Further recrystallization from ethyl acetate/hexane affords an analytical sample: m.p. 78°-85° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04243674 |
| 출처 데이터셋 | uspto-grants-1981_01 |
| ORD ID | ord-0decae391ec24e7f9a84a79f28035cc6 |
| 출처 메모 | uspto-grants-1981_01 |