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Sulfuric Acid → 4-(7,12-Dihydroxy-3-methanesulfonyloxy-10,13-dimethylhexadecahydrocyclopenta[a]phenanthren-17-yl) pentanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Cholic Acid | HCID 221493 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 4-(7,12-Dihydroxy-3-methanesulfonyloxy-10,13-dimethylhexadecahydrocyclopenta[a]phenanthren-17-yl) pentanoic acid | HCID 18425131 | — |
反応手順
100 g of cholic acid are dissolved in 500 ml of pyridine and 23.1 ml of mesyl chloride are added dropwise over a period of 30 minutes at 0° C. The mixture is stirred at RT for 3 hours, then poured into a solution of 400 ml of H2SO4 in 3 l of water at 0° C. and extracted 4 times using 750 ml of EA each time. The extract 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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06451781B1 |
| 出典データセット | uspto-grants-2002_09 |
| ORD ID | ord-9cf26ad6bde54e74befc09eb17913f95 |
| 出典メモ | uspto-grants-2002_09 |