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 | 2-Amino-3-methylpyridine | HCID 15347 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | Metaperiodic acid | HCID 65185 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Iodo-3-methylpyridin-2-amine | HCID 959586 | 174.9% |
反応手順
To a solution of 3-methyl-2-pyridineamine (10 g) in a mixed solution of AcOH (60 mL), water (12 mL), and sulfuric acid (4.2 mL) was added periodic acid dehydrate (4.22 g) and iodine (9.39 g), and the mixture was heated at 80° C. for 2 hours. The reaction mixture was poured into 5% Na2S2O3 aq solution and extracted with ether. The organic layer was washed with 1N NaOH aq solution and brine, and dried over Na2SO4. The solvent was removed in vacuo and obtained residual solid was recrystallized with EtOH to give 5-iodo-3-methyl-2-pyridinamine (9.00 g) as pale yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07557127B2 |
|---|
| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-53f55ca96c1d4c3cab9aef891b414de3 |
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| 出典メモ | uspto-grants-2009_07 |
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