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5-Chloro-salicylaldehyde → 5-Chloro-2-hydroxy-3-iodobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 5-Chloro-salicylaldehyde | HCID 12481 | — |
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-Chloro-2-hydroxy-3-iodobenzaldehyde | HCID 3772545 | 90% |
反応手順
N-Iodosuccinimide (144.0 g, 0.641 mole) was added to a solution of 5-chlorosalicylaldehyde (100 g, 0.638 mole) in dimethylformamide (400 mL). The reaction mixture was stirred for 2 days at room temperature. Additional N-iodosuccinimide (20.0 g) was added and the stirring was continued for an additional 2 days. The reaction mixture was diluted with ethyl acetate (1 L), washed with hydrochloric acid (300 mL, 0.1N), water (300 mL), sodium thiosulfate (5%, 300 mL), brine (300 mL), dried (MgSO4) and was concentrated to dryness to afford the desired aldehyde (162 g, 90% yield) as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06372719B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-53bb324b60ff48b980b9629dbc3566a2 |
| 出典メモ | uspto-grants-2002_04 |