関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Glycidol | HCID 11164 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 5-Acetamido-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide | HCID 11115326 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | 2-Methoxyethanol | HCID 8019 | — |
| 生成物 | Iohexol | HCID 3730 | 64.6% |
反応手順
5.0 gram 5-acetamino-N,N'-bis-(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzene-dicarboxamide (Compound 1), 0.36 gram of 25% sodium methoxide in methanol, and 1.5 gram glycidol are combined in 2-methoxyethanol and heated to 90° C. for four hours. Solvent is removed under vacuum followed by dissolution of the residue in water. The solution is treated with 1 gram each of Amberlyst A-15 and Amberlite IRA-67 ion-exchange resins to remove sodium methoxide. Water is removed under vacuum to afford an oil. Crystallization from methanol/isopropanol (10:75) afforded 3.5 gram (64.6%) iohexol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05847212 |
|---|
| 出典データセット | uspto-grants-1998_12 |
|---|
| ORD ID | ord-04ece25d1e684e0ca9e702346e883205 |
|---|
| 出典メモ | uspto-grants-1998_12 |
|---|
