反応式
O.NN.[OH-].[K+].O=[C:7]([C:16]1[CH:20]=[CH:19][S:18][CH:17]=1)[CH2:8][CH:9](C(O)=O)[C:10]([OH:12])=[O:11].Cl.[Na+].[Cl-]>C(O)CO>[S:18]1[CH:19]=[CH:20][C:16]([CH2:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[CH:17]1参加物
7
実験手順
Hydrazine hydrate (1.3 mL, 1.34 g, 26.8 mmol) was added dropwise to a solution of KOH (3.54 g, 63 mmol) and 2-[2-oxo-2-(3-thienyl) ethyl] malonic acid 8(c) (4.00 g, 17.5 mmol) in ethylene glycol (30 mL). This solution was heated at reflux for 6 hours. After cooling to room temperature, the crude reaction mixture was poured into a mixture of 6N HCl (50 mL) and ice (200 g). This aqueous mixture was saturated with NaCl, then extracted with ether (3×70 mL). The combined organic extracts were dried over Na2SO4 and concentrated, in vacuo, to provide an orange oil (2.61 g) of sufficient purity to be employed in the-subsequent reaction without any further purification.
後処理
- temperatureThis solution was heated
- temperatureat reflux for 6 hours
- customthe crude reaction mixture
- extractionextracted with ether (3×70 mL)
- dry with materialThe combined organic extracts were dried over Na2SO4
- concentrationconcentrated, in vacuo
出典と根拠
- ORDレコード
- ord-0f3cc0721c0a4572b7d98b75e8c1ae33
- 出典データセット
- uspto-grants-1999_08
- 特許番号
- US05945427
関連ノート
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