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Hydrochloric Acid → 5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Tetraacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide | HCID 10395011 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Tetraacetate | HCID 9897534 | — |
反応手順
5-Amino-2,4,6-triiodo-N,N'-bis(2,3-dihydroxypropyl)-isophthalamide (14.08 g, 0.02 mol), which had been prepared according to GB-A-1548594 was suspended in pyridine (200 ml) and acetic anhydride (57.1 g, 0.56 mol) was added dropwise with stirring and cooling. After stirring overnight, the mixture was poured into ethyl acetate (300 ml) and 20% aqueous HCl (200 ml). After extraction, the organic phase was washed with 2 M aqueous HCl (20 ml), brine (70 ml), dried (Na2SO4) and evaporated. Yield 17.4 g (100%). The crude material was used without further purification, since analysis by HPLC and 1H NMR indicated, that the product was >97% pure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05958376 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-1ea3159e0afd4efbb1c41f863e2be904 |
| 出典メモ | uspto-grants-1999_09 |