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Citric Acid → HCID 68207887、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | Methyl 4-aminobenzoate | HCID 12082 | — |
| 反応物 | 2-(Trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate | HCID 86676334 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 68207887 | HCID 68207887 | 88.5% |
反応手順
To a mixture of 1.04 g of 2-(trimethylsilyl)ethyl 3-(chlorosulfonyl)benzoate and 10 mL of pyridine was added 512 mg of methyl 4-aminobenzoate, followed by stirring at room temperature for 1 hour. To the reaction mixture was added a 10% aqueous citric acid solution, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to obtain 1.25 g of 2-(trimethylsilyl)ethyl 3-{[4-(methoxycarbonyl)phenyl]sulfamoyl}benzoate as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09284295B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-6866aa2cc2e14945a95ad33fb99c94c3 |
| 出典メモ | uspto-grants-2016_03 |