Acetic Anhydride → Gestodene Impurity 1
反応式
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].O[C@@H]1[C@H:15]2[C@H:16]3[C@H:25]([CH2:26][CH2:27][C@:12]2([CH2:13][CH3:14])[C:11](=[O:29])C1)[C@@H:24]1[C:19](=[CH:20][C:21](=[O:28])[CH2:22][CH2:23]1)[CH2:18][CH2:17]3>N1C=CC=CC=1>[C:5]([O:4][C@@H:1]1[C@H:15]2[C@H:16]3[C@H:25]([CH2:26][CH2:27][C@:12]2([CH2:13][CH3:14])[C:11](=[O:29])[CH2:2]1)[C@@H:24]1[C:19](=[CH:20][C:21](=[O:28])[CH2:22][CH2:23]1)[CH2:18][CH2:17]3)(=[O:7])[CH3:6]参加物
4
実験手順
200 ml of acetic anhydride is added dropwise to 100 g of 15α-hydroxy-18-methyl-4-estrene-3,17-dione in 350 ml of pyridine. After one hour, the reaction mixture is stirred into ice water. The thus-precipitated product is suctioned off, washed neutral with water, and dried under vacuum at 50° C., thus obtaining 100 g of 15α-acetoxy-18-methyl-4-estrene-3,17-dione. A sample recrystallized from acetone/hexane melts at 165° C.