関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | 3-Nitropyridin-2-ylamine | HCID 77887 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Amino-5-iodo-3-nitropyridine | HCID 3384468 | 193.8% |
反応手順
A mixture of 2-amino-3-nitropyridine (5.0 g, 35.9 mmol), acetic acid (22 mL), water (5 mL), sulfuric acid (0.650 mL), and HIO4×2H2O (1.7 g, 7.5 mmol) was allowed to stir at 90° C. for 10 min. Iodine crystals (3.7 g, 14.6 mmol) were added in portions. After stirring for 1 h, the reaction was poured into saturated sodium thiosulfate and extracted with ethyl acetate. The organic layers were washed with 0.1 M NaOH and saturated brine, dried with sodium sulfate, then evaporated to give orange solid (7.5 g, 79% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07615567B2 |
|---|
| 出典データセット | uspto-grants-2009_11 |
|---|
| ORD ID | ord-fffef87291884d818b0849cb29e0c2af |
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| 出典メモ | uspto-grants-2009_11 |
|---|
