反応式
[C:1]([C:4]1[CH:8]=[CH:7][S:6][CH:5]=1)(=[O:3])[CH3:2].[O:9]1CCOCC1>O>[S:6]1[CH:7]=[CH:8][C:4]([C:1]([CH:2]=[O:9])=[O:3])=[CH:5]1参加物
実験手順
3-Acetylthiophene (20.0 g., 0.159 mol) and SeO2 (19.4 g., 0.175 mol) were dissolved 100 ml. dioxane and 8 ml. H2O by warming to 35°, then heated at reflux 16 hours. The reaction mixture was cooled, filtered and the filtrate stripped to a sludge (the hydrate of title product in crude form). The latter was distilled at reduced pressure to yield title product contaminated with about 10% starting material, 8.53 g.; tlc (5:3 hexane:ethyl acetate) Rf 0.27 (title product) and 0.59 (3-acetylthiophene). The latter was chromatographed on silica gel with 5:3 hexane:ethyl acetate as eluant. Clean product fractions were combined stripped to a solid, triturated with hexane, filtered and the solids (5.60 g.) sublimed to yield purified title product, 3.20 g.; tlc Rf 0.27 as above; sublimation point 70°/1 mm; ms: parent 141, base 111.
後処理
- temperatureheated
- temperatureat reflux 16 hours
- temperatureThe reaction mixture was cooled
- filtrationfiltered
- distillationThe latter was distilled at reduced pressure
出典と根拠
- ORDレコード
- ord-e9a92da5722a47b1aacce5c45a323492
- 出典データセット
- uspto-grants-1987_06
- 特許番号
- US04675186
関連ノート
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