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Sodium Carbonate → 3-Iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 3-Iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine | HCID 57900211 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine 1-oxide | HCID 58284041 | 96.3% |
反応手順
m-Chloroperbenzoic acid (1.55 g, 6.29 mmol) was added portionwise to a solution of 1.0 g (3.02 mmol) of 3-iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine in 150 ml of methylene chloride. The mixture was stirred for 18 hours then mixed with 100 ml of 1 M aqueous sodium carbonate. The organic layer was separated and the aqueous one was extracted 2 times with 10 ml of methylene chloride. Combined organic extracts were washed with brine and dried over sodium sulfate. The solution was concentrated in vacuum to give 3-iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine 1-oxide (1.01 g, 92%). MS: (ESI+) 348.0
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09309265B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-bb7485e41aca4e91974363d6d971d27c |
| 出典メモ | uspto-grants-2016_04 |