関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Iodic acid | HCID 24345 | — |
| 反応物 | 4-(4-Methoxyphenyl)pyrrolidin-2-one | HCID 4656224 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 4-(3-Iodo-4-methoxyphenyl)pyrrolidin-2-one | HCID 14529699 | 414.5% |
反応手順
A solution of 19.1 g of 4-(4-methoxyphenyl)-pyrrolidin-2-one (100 mmol) in 200 ml of glacial acetic acid, 4.8 ml of water and 1.2 ml of concentrated sulfuric acid is combined with 3.44 g (19.55 mmol) of iodic acid and 8.64 g (70 mmol) of iodine and stirred at a bath temperature of 80° C. for 10 hours. Subsequently, the mixture is concentrated on a rotary evaporator up to onset of crystallization, cooled, the crystalline precipitate is suctioned off and recrystallized from ethyl acetate, thus obtaining 25.7 g (81% of theory) of 4-(3-iodo-4-methoxyphenyl)pyrrolidin-2-one, mp 158° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05064854 |
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| 出典データセット | uspto-grants-1991_11 |
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| ORD ID | ord-26c59e9504d54bb5a2e995bb7b7c6dd0 |
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| 出典メモ | uspto-grants-1991_11 |
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