関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2-Chloropropionyl chloride | HCID 111019 | — |
| 反応物 | (+/-)-(3R,4S)-3-hydroxy-4-methylcarbonyloxytetrahydrofuran | HCID 22883851 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (+/-)-(3R,4S)-4-Acetoxy-3-(2-chloropropionyloxy)tetrahydrofuran | HCID 15789790 | — |
反応手順
12.4 g of (±)-2-chloropropionyl chloride were added dropwise at 0°-5° C. to an ice-cooled mixture of 15.0 g of (±)-(3R,4S)-3-hydroxy-4-methylcarbonyloxytetrahydrofuran, 8.1 g of anhydrous pyridine and 200 ml of anhydrous dichloromethane. After addition was complete, the reaction mixture was stirred at 23° C. for a further 4 hours, after which it was poured onto 400 ml of water. The organic phase was then separated off, washed twice with 50 ml of water each time, dried over sodium sulfate and finally concentrated. The crude product was purified by distillation at a pressure of 10 mbar.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05733850 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-e6001659ddac4b01bf370c708fa8cdd0 |
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| 出典メモ | uspto-grants-1998_03 |
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