関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 1,3-Dimethyl-2-imidazolidinone | HCID 6661 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 溶媒 | 7-Ketolithocholic acid | HCID 444262 | — |
| 生成物 | 1,3-Dimethyl-2-imidazolinone Ethanol | HCID 70473090 | — |
反応手順
In an undivided flow-through cell with ruthenized titatium anode and cathode, 1.95 g of 7-ketolithocholic acid was dissolved in an electrolyte made from 0.65 g of lithium chloride, 60 mL of 1,3-dimethyl 2-imidazolidinone and 200 mL of absolute ethanol. The solution in both the cell and the reservoir was kept under nitrogen. Initially, current of up to 4 amperes were passed through the cell but polarization occurred and the current had to be reduced to 400 ma. Electrolysis was continued until 97 coulombs had been delivered. The solvent was removed under high vacuum, and the residue dissolved in 2N sodium hydroxide. The product was precipitated by adding this alkaline solution dropwise to acidic (pH 2.0) water. The recovery was 76.9%. The percent reduction was 36.8. The ratio of ursodeoxycholic acid to chenodeoxycholic acid was 1.45.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04547271 |
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| 出典データセット | uspto-grants-1985_10 |
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| ORD ID | ord-0d10ef6b44a54d52871ca9343fea3dbf |
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| 出典メモ | uspto-grants-1985_10 |
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