반응 #57423
ord-f6134be461a14511880bb3bc6c707851
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후처리
- 1기타is prepared
- 2기타at ambient temperature
- 3기타has been completely consumed
- 4온도The reaction medium is maintained
- 5농축The reaction medium is subsequently concentrated under vacuum
- 6기타The crude reaction product
- 7기타is obtained
- 8추출The resulting aqueous phase is extracted with ethyl acetate (3×300 mL)
- 9건조dried over MgSO4
- 10농축concentrated under vacuum
- 11기타The crude reaction product
- 12기타is dried under vacuum
- 13기타to give
실험 절차
In a 2-liter three-neck round-bottom flask equipped with a dropping funnel and a paddle stirrer a solution of sodium ethoxide is prepared by reacting metallic sodium (7.74 g, 340.00 mmol, 1.2 eq) in anhydrous ethanol (800 ml) at ambient temperature until the metallic sodium has been completely consumed. A solution of diethyl oxalate (37.20 mL, 280.00 mmol, 1.0 eq) in acetone (10.30 mL, 280.00 mmol, 1.0 eq) is subsequently added dropwise at ambient temperature. The reaction medium is maintained with vigorous stirring for 2 hours. The reaction medium is subsequently concentrated under vacuum. The crude reaction product is diluted in water (200 ml). Ice (100 g) is added, followed by concentrated sulfuric acid (20 ml) in small portions, until a clear orange solution is obtained. The resulting aqueous phase is extracted with ethyl acetate (3×300 mL). The organic phases are combined, dried over MgSO4 and then concentrated under vacuum. The crude reaction product is dried under vacuum to give, quantitatively, the expected product (m=44.71 g).