Water → 2-Furylmalonic acid diethyl ester

HRID 1655758

반응식

HRID 1655758 반응식
CO[CH:3]1[CH:7]=[CH:6][CH:5](OC)[O:4]1.[CH2:10]([O:12][C:13](=[O:20])[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH3:11].O>[Cl-].[Zn+2].[Cl-].C(O)(=O)C>[CH2:10]([O:12][C:13](=[O:20])[CH:14]([C:5]1[O:4][CH:3]=[CH:7][CH:6]=1)[C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH3:11]

참가 물질

6

반응물 3

HCID 962WaterHCID 7761Diethyl MalonateHCID 789742,5-Dihydro-2,5-dimethoxyfuran

생성물 1

HCID 128365772-Furylmalonic acid diethyl ester수율 29%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 176Acetic Acid용매

실험 절차

340 g (2.5 mmol) of zinc chloride were added in one portion to a solution of 217 g (1.67 mol) of 2,5-dimethoxy-2,5-dihydrofuran, 1500 ml (10 mol) of malonic acid diethyl ester, 167 ml of Water and 330 ml of glacial acetic acid. The temperature rose to 35°. The dark solution was stirred at room temperature overnight, poured onto ice, extracted three times with diethyl ether, washed in succession with saturated sodium bicarbonate and sodium chloride solutions, and finally dried. After evaporating the excess malonic acid diethyl ester (70°/13 Pa), the remaining oil was distilled over a Vigreux column, to obtain 109.2 g (29%) of 2-furylmalonic acid diethyl ester (purity 94%), boiling point 100°-110°/39 Pa.

후처리

  1. customrose to 35°
  2. additionpoured onto ice
  3. extractionextracted three times with diethyl ether
  4. washwashed in succession with saturated sodium bicarbonate and sodium chloride solutions
  5. customfinally dried
  6. customAfter evaporating the excess malonic acid diethyl ester (70°/13 Pa)
  7. distillationthe remaining oil was distilled over a Vigreux column

출처 및 근거

ORD 기록
ord-a84ce0c2384f46d9a1b1262447ac2d9e
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250517

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