関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexylene Glycol | HCID 7870 | — |
| 反応物 | HCID 178496632 | HCID 178496632 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Temsirolimus | HCID 6918289 | — |
反応手順
Crude CCI-779 was prepared essentially as described above from CCI-779 boronate using 5 eq. of 2-methyl-2,4-pentanediol in a mixture of ether and heptanes (2:1, Wt/Wt) at 34° C. for 6 hours. The crude CCI-779 was isolated by filtration. The crude CCI-779 was suspended in ether, then treated with 5 eq. of 2-methyl-2,4-pentanediol, following by addition of heptanes, filtration, and drying. The dried, partially purified CCI-779 is then dissolved in acetone, clarified, and acetone removed. Following this, ether is added to crystallize product, heptanes added to the ether slurry, the slurry is filtered and dried. The resulting yield is 73% of CCI-779, having a strength of 93.5%, total impurities of less than 4% (i.e., 3.59%), and significantly, PhB(OH)2 of 0.007.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07622578B2 |
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| 出典データセット | uspto-grants-2009_11 |
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| ORD ID | ord-4f059e7ed6f74825a78436afc8eed242 |
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| 出典メモ | uspto-grants-2009_11 |
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