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Potassium Carbonate → HCID 16782287、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Picolyl chloride hydrochloride | HCID 23392 | — |
| 反応物 | 4-Mercaptobenzoic acid | HCID 95738 | — |
| 溶媒 | Water ethanol | HCID 19096565 | — |
| 生成物 | HCID 16782287 | HCID 16782287 | 40.9% |
反応手順
An ethanol/water mixed solution (2/1, 60 mL) of 4-mercaptobenzenecarboxylic acid (1.0 g), 2-chloromethylpyridine hydrochloride (2.1 g) and potassium carbonate (4.5 g) was heated under reflux for 4 hours. The organic solvent was evaporated off under reduced pressure, and aqueous 5 N hydrochloric acid solution was added to the residue until it became acidic. Water was evaporated off under reduced pressure, and DMF was added to the resulting residue and filtered. The filtrate was concentrated under reduced pressure, and the resulting residue was purified through silica gel column chromatography (chloroform/methanol=9/1 to 4/1) to obtain the entitled compound (650 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07566781B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-e616d6cef73c4db7ba90b40ae60674af |
| 出典メモ | uspto-grants-2009_07 |