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Hydrochloric Acid → 4-Chloro-2-fluoro-5-methoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Formate | HCID 2723810 | — |
| 反応物 | 1-Chloro-5-fluoro-4-iodo-2-methoxybenzene | HCID 22625607 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Chloro-2-fluoro-5-methoxybenzaldehyde | HCID 14928268 | 30% |
反応手順
A mixture of 36.3 g of 2-chloro-4-fluoro-5-iodo-1-methoxybenzene, 12.9 g of sodium formate, 1.78 g of dichlorobis(triphenylphosphine) palladium, and 113 ml of N,N-dimethylformamide was stirred, while bubbling carbon monoxide at 90° to 100° C. over 12 hours. After completion of the reaction, the reaction mixture was returned to room temperature, followed by dilution with diluted hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography, which afforded 7.09 g (yield, 30%) of 4-chloro-2-fluoro-5-methoxybenzaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06015774 |
| 出典データセット | uspto-grants-2000_01 |
| ORD ID | ord-43c7107112214bd38503012d6044da09 |
| 出典メモ | uspto-grants-2000_01 |