関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Calcium Carbonate | HCID 10112 | — |
| 反応物 | 4-Chloromethyl-N-(2-methoxyphenyl)benzamide | HCID 19689968 | — |
| 反応物 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Hydroxymethyl-N-(2-methoxyphenyl)benzamide | HCID 4792000 | 88.3% |
反応手順
4-Chloromethyl-N-(2-methoxyphenyl)benzamide (500 mg, 1.81 mmol) and precipitated calcium carbonate (970 mg, 9.7 mmol) were suspended in a dioxane-water (1:1) mixture solution (9 ml) and subjected to 25 hours of heating under reflux. After adding THF (25 ml) and filtering off the formed insoluble materials, the organic solvent was removed by evaporation. The thus obtained residue was extracted with ethyl acetate, and the resulting organic layer was washed with saturated brine and dried on anhydrous magnesium sulfate. After removing the solvent by evaporation, the resulting colorless solid material was purified by subjecting it to a silica gel column chromatography (ether:hexane=3:1), thereby obtaining 411 mg (88.3%) of the title compound in the form of colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728835 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-721576edcf544abdbf97d483a0968b14 |
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| 出典メモ | uspto-grants-1998_03 |
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