関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 6-Chloro-5-methylpyridine-3-carbaldehyde | HCID 19710681 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Chloro-5-methylnicotinic acid | HCID 12387729 | — |
反応手順
A solution of 6-chloro-3-formyl-5-methyl-pyridine (10 g, 64 mmol) in formic acid (200 mL) is cooled at 0° C. and an aq. 50% wt solution of H2O2 in water (9.6 mL, 360 mmol) is added at this temperature. The mixture is stirred at 0° C. for 15 h, carefully diluted with water (200 mL) and extracted with DCM (8×100 mL). The combined org. extracts are washed with 1M aq. HCl (100 mL) (check for remaining peroxide), dried (MgSO4), filtered and evaporated. The residue is dried to give 6-chloro-5-methyl-nicotinic acid (9.56 g); LC-MS: tR=0.72 min, [M+1]+=172.0.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08288554B2 |
|---|
| 出典データセット | uspto-grants-2012_10 |
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| ORD ID | ord-d11d72e279474c9cb5f9114e16d8b78d |
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| 出典メモ | uspto-grants-2012_10 |
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