反応式
[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C:12]4[CH:13]=[CH:14][C:15]([O:20]C)=[CH:16][C:17]=4[CH2:18][CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C@@H:4]2[OH:22])[CH3:2].N.[Li]>O.O1CCCC1.C(O)C>[CH2:1]([C@:3]12[CH2:11][CH2:10][C@@H:9]3[C@@H:12]4[C:17]([CH2:18][CH2:19][C@H:8]3[C@@H:7]1[CH2:6][CH2:5][C@@H:4]2[OH:22])=[CH:16][C:15](=[O:20])[CH2:14][CH2:13]4)[CH3:2]参加物
7
実験手順
Add 13β-ethyl-3-methoxy-gona-1,3,5(10)-trien-17β-ol (0.5 g.) in 100 ml. of tetrahydrofuran to 150 ml. of liquid ammonia, followed by 0.5 g. of lithium foil, and stir the mixture for 10 minutes. Add ethanol (6 ml.) and tetrahydrofuran (10 ml.) over a period of 20 minutes. After disappearance of the blue color add water, extract the mixture well with ether and evaporate the washed and dried ether extract. Dissolve the crystalline residue in 50 ml. of methanol and reflux for 30 minutes with 30 ml. of 3N HCL. Remove most of the methanol under reduced pressure, and extract the residue with ether. Chromatograph the ether extract on alumina. Use benzene-ether (1:1) to elute 13-β-ethyl-17β-hydroxy-gon-4-en-3-one; m.p. 152°-55° C.
後処理
- extractionextract the mixture well with ether
- customevaporate the
- washwashed
- extractiondried ether extract
- dissolutionDissolve the crystalline residue in 50 ml
- temperatureof methanol and reflux for 30 minutes with 30 ml
- customRemove most of the methanol under reduced pressure
- extractionextract the residue with ether
- extractionChromatograph the ether extract on alumina
- washto elute 13-β-ethyl-17β-hydroxy-gon-4-en-3-one
出典と根拠
- ORDレコード
- ord-6727c76ff08c4185bcd15a7d11b6cf86
- 出典データセット
- uspto-grants-1976_05
- 特許番号
- US03959322
関連ノート
読み込み中…