関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfamic Acid | HCID 5987 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | Monobasic potassium phosphate | HCID 516951 | — |
| 反応物 | Sodium Chlorite | HCID 23668197 | — |
| 反応物 | 5-Formyl-2-furancarboxylic acid benzyl ester | HCID 60034788 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Furan-2,5-dicarboxylic Acid Monobenzyl Ester | HCID 16091220 | 99.2% |
反応手順
490 mg of 5-formylfuran-2-carboxylic acid benzyl ester was dissolved in 10 mL of acetonitrile, and added with a solution containing 413 mg of sulfamic acid in 5 mL of water. After cooling to 0° C., a solution containing 202 mg of sodium chlorite and 232 mg of potassium dihydrogen phosphate in 5 mL of water was added dropwise. After cooling at this temperature for 30 minutes, sodium thiosulfate aqueous solution was added at 0° C. to stop the reaction, and extracted with a mixture of tetrahydrofuran and ethyl acetate. The organic phase was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off to afford 520 mg of the title compound as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07429609B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-c6f74879b55d4a9f9448b3912936560b |
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| 出典メモ | uspto-grants-2008_09 |
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