Ethylene Glycol → HCID 14547485、化合物
反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[CH:11]=[CH:10][S:9][C:8]=2[CH:12]=1)(=[O:3])[CH3:2].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:24](O)[CH2:25][OH:26].O>C1(C)C=CC=CC=1>[CH3:2][C:1]1([C:4]2[CH:5]=[CH:6][C:7]3[CH:11]=[CH:10][S:9][C:8]=3[CH:12]=2)[O:26][CH2:25][CH2:24][O:3]1参加物
6
実験手順
A mixture of 6-acetyl benzo[b]thiophene (10.57 g, 60 mmole), p-toluenesulfonic acid (1.65 g) and ethylene glycol (33 ml) was heated to reflux in toluene (250 ml) for 2 hours with the continuous removal of H2O using a Dean-Stark trap. The reaction mixture was allowed to cool to room temperature. Then extracted with 20% saturated NaHCO3 (150 ml) and H2O (2×150 ml). After drying over Na2SO4, the solvent was evaporated in vacuo and the residue was crystallized from hexanes (50 ml) yielding 9.66 g (73%) of product.
後処理
- temperaturewas heated
- extractionThen extracted with 20% saturated NaHCO3 (150 ml) and H2O (2×150 ml)
- dry with materialAfter drying over Na2SO4
- customthe solvent was evaporated in vacuo
- customthe residue was crystallized from hexanes (50 ml)
出典と根拠
- ORDレコード
- ord-302f70c0cdc448cc86c3513ca0830242
- 出典データセット
- uspto-grants-1987_05
- 特許番号
- US04668697
反応ノート
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