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Pyridine → 17-Methylenestra-1,3,5(10)-trien-3-yl acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 17-Methylene-estra-1,3,5(10)-trien-3-ol | HCID 14458552 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 17-Methylenestra-1,3,5(10)-trien-3-yl acetate | HCID 18642305 | — |
反応手順
A solution of 17-methylenestra-1,3,5(10)-trien-3-ol (10, 5.84 g, 21.8 mmol) in anh. pyridine (32 ml, 0.40 mol) and acetic anhydride (9.7 ml, 0.10 mol) was stirred 24, after which ethyl acetate (250 ml) was added. See FIG. 160. The mixture was washed with three 100 ml portions of 1 N hydrochloric acid+100 ml of saturated sodium bicarbonate+100 ml of saturated copper sulfate+100 ml of brine, dried over magnesium sulfate, and filtered through diatomaceous earth. The residue was washed with 25 ml of ethyl acetate and the combined filtrates were concentrated under reduced pressure. Recrystallization from aqueous ethanol gave lustrous white platelets (5.84 g, 18.8 mmol), m.p. 77-79° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06057439 |
| 出典データセット | uspto-grants-2000_05 |
| ORD ID | ord-eaadba33f09d44d5a02af13033641f58 |
| 出典メモ | uspto-grants-2000_05 |