関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-(2,4-Difluorophenyl)-1,2,3-propanetriol | HCID 11217952 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 1,3-Diacetoxy-2-(2,4-difluorophenyl)-2-propanol | HCID 15463462 | — |
反応手順
In 100 ml of pyridine was dissolved 10 g of 2-(2,4-difluorophenyl)-1,2,3-propanetriol. To the resulting solution was added dropwise 1.1 g of acetic anhydride at room temperature. After the dropping, the resulting liquid was stirred at room temperature for 1 hour. Then, to the reactiom mixture was added 50 ml of ethyl acetate, and an organic layer was separated therefrom. After the organic layer was washed with 1N aqueous solution of hydrochloric acid and further washed with water and saturated aqueous solution with sodium chloride. Then the organic layer was dried over anhydrous sodium sulfate. The resulting organic layer was filtered and the solvent was removed under reduced pressure. Thus obtained concentrate was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1) to give 12.5 g of the desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05840553 |
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| 出典データセット | uspto-grants-1998_11 |
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| ORD ID | ord-4bbd2f00e09d4caab222fa68732a9815 |
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| 出典メモ | uspto-grants-1998_11 |
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