Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 4-(7,12-Dihydroxy-3-methanesulfonyloxy-10,13-dimethylhexadecahydrocyclopenta[a]phenanthren-17-yl) pentanoic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | Cholic Acid | HCID 221493 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | 4-(7,12-Dihydroxy-3-methanesulfonyloxy-10,13-dimethylhexadecahydrocyclopenta[a]phenanthren-17-yl) pentanoic acid | HCID 18425131 | — |
반응 단계
100 g of cholic acid are dissolved in 500 ml of pyridine and 23.1 ml of mesyl chloride are added dropwise at 0° C. over a period of 30 minutes. The mixture is stirred at RT for 3 hours, then poured onto a solution of 400 ml of H2SO4 in 3 l of water at 0° C. and extracted 4 times with 750 ml of EA each time. The organic phase is dried over Na2SO4 and the solvent is removed in vacuo. The residue is crystallized using diisopropyl ether and 117.1 g are obtained; m.p. 121° C. (with decomposition). Rf (EA/HEP/acetic acid 5:5:1)=0.31 MS (FAB): 487 (M+H)+
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06166002 |
| 출처 데이터셋 | uspto-grants-2000_12 |
| ORD ID | ord-4bb7fd5933aa45639c928c5bb31f2603 |
| 출처 메모 | uspto-grants-2000_12 |