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2,2,2-Trifluoroethyl butanoate → 17alpha-Hydroxy-21-butanoyloxy-pregna-4,9(11)-diene-3,20-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2,2-Trifluoroethyl butanoate | HCID 193290 | — |
| 反応物 | Anecortave | HCID 7074810 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 17alpha-Hydroxy-21-butanoyloxy-pregna-4,9(11)-diene-3,20-dione | HCID 86720232 | — |
反応手順
A mixture of 1 g (2.879 mM) of 17α,21-dihydroxy-pregna-4,9(11)-diene-3,20-dione and 10 ml of trifluoroethyl butanoate in 100 ml of acetone was reacted at 45° C. in the presence of 5 g of Candida cylindracea lipase for 8-10 hours, adding 1 g of lipase at regular time intervals. After completion of the reaction, the lipase was filtered off and the filtrate was concentrated under vacuum, taking up the residue three times with acetone. The semi-solid residue was purified by chromatography on a silica gel column with a dichloromethane/methanol 99:1 mixture. The less polar components were removed, to obtain the richer fraction which was evaporated to yield 0.95 g (2.29 mM) of 17α-hydroxy-21-butanoyloxy-pregna-4,9(11)-diene-3,20-dione.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865690B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-b02d7551d0684fd2b2feceb34728a024 |
| 出典メモ | uspto-grants-2014_10 |