関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 3-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline | HCID 18429181 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-acetyl-3-acetoxymethyl-5-(2,3-diacetoxypropylaminocarbonyl)-2,4,6-triiodoaniline | HCID 18429152 | — |
反応手順
3-Hydroxymethyl-5-(2,3-dihydroxypropylaminocarbonyl)-2,4,6-triiodoaniline (3.3 g, 5.3 mmol) was suspended in glacial acetic acid (12 ml) containing acetic anhydride (48 ml) and concentrated sulfuric acid (0.08 ml). The mixture was stirred at 60° C. for 3 h, allowed to cool to room temperature, and CH2Cl2 (100 ml) and water (100 ml) were added. The organic phase was washed with water (3×50 ml) and a saturated aqueous solution of NaHCO3 (2×50 ml). After drying (MgSO4) and evaporation, the residue was dissolved in a mixture of CH2Cl2 and methanol (9:1) and filtered through a short silica pad and evaporated. Yield: 3.0 g (71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05993780 |
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| 出典データセット | uspto-grants-1999_11 |
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| ORD ID | ord-05afd05decce4072978c122a9b58c864 |
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| 出典メモ | uspto-grants-1999_11 |
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