関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-methoxy-2,5-dihydro-1H-pyrrol-2-one | HCID 574769 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Benzyloxy-3-pyrrolin-2-one | HCID 2724741 | — |
反応手順
5.7 g of 4-methoxy-3-pyrrolin-2-one and 10.8 g of benzyl alcohol were mixed with 0.4 g of methane sulfonic acid and stirred for 24 hours at 80° C. and 20 mbars. Then the reaction solution was mixed with 50 ml of ice water and 100 ml of methylene chloride and neutralized with 4 ml of saturated NaHCO3 solution. The aqueous phase was extracted twice more with 50 ml each of methylene chloride. After drying of the organic phase over Na2SO4 and distilling off of the solvent, the residue was mixed with 150 ml of ice water, heated to 100° C. and 100 ml of water-benzyl alcohol was azeotropically distilled off. The crystals precipitated during the cooling were recrystallized hot from 50 ml of toluene. 6.7 g of white, crystalline product with a melting point of 147° to 148° was obtained. For the product:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04849528 |
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| 出典データセット | uspto-grants-1989_07 |
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| ORD ID | ord-8caa1fe527544a2e9c53fbfaa7fadd98 |
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| 出典メモ | uspto-grants-1989_07 |
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