関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Chlorotriethylsilane | HCID 13819 | — |
| 反応物 | 10-deacetylbaccatin III | HCID 154272 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 7-O-(Triethylsilyl) Baccatin III | HCID 9939927 | 77% |
反応手順
182 g of triethylsilyl chloride are added over 1 hour 20 minutes to a solution of 293.9 g of 10-deacetylbaccatin III in 2.7 liters of pyridine. The solution obtained is stirred for 40 hours at 5° C. 360 g of acetic anhydride are then added while the temperature is maintained at 5° C. The suspension obtained is stirred for 48 hours at 20° C. and then poured into 40 liters of ice-cold water. The precipitate obtained is separated by filtration, then washed with 8 times 2 liters of water and lastly dissolved in 3 liters of ethyl acetate. The organic phase is dried over magnesium sulphate. After filtration and concentration under reduced pressure, the product obtained is crystallized in isopropyl ether. 7-(Triethylsilyl)baccatin III is thereby obtained in a 77% yield, the characteristics of which product are as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05959125 |
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| 出典データセット | uspto-grants-1999_09 |
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| ORD ID | ord-64b6443b641f4ba481be1bfbe1569598 |
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| 出典メモ | uspto-grants-1999_09 |
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