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Chloroform → Methyl 4-{[2-oxodihydro-3(2H)-furanylidene]methyl}benzoate

HRID 2243286
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HRID 2243286 반응식
C1(P(C2C=CC=CC=2)(C2C=CC=CC=2)=[C:8]2[CH2:12][CH2:11][O:10][C:9]2=[O:13])C=CC=CC=1.[CH:26]([C:28]1[CH:37]=[CH:36][C:31]([C:32]([O:34][CH3:35])=[O:33])=[CH:30][CH:29]=1)=O.C(Cl)(Cl)Cl>CS(C)=O>[O:13]=[C:9]1[C:8](=[CH:26][C:28]2[CH:37]=[CH:36][C:31]([C:32]([O:34][CH3:35])=[O:33])=[CH:30][CH:29]=2)[CH2:12][CH2:11][O:10]1
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참가 물질

5

반응물 3

HCID 6212ChloroformHCID 15294Methyl 4-FormylbenzoateHCID 971112(3H)-Furanone, 3-(triphenylphosphoranylidene)-

생성물 1

HCID 68707654Methyl 4-{[2-oxodihydro-3(2H)-furanylidene]methyl}benzoate

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

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온도
80 °C

실험 절차

A mixture of 40.00 g (0.12 mol) of 3-(triphenylphosphoranylidene)dihydro-2(3H)-furanone and 20.85 g (0.13 mol) of methyl 4-formylbenzoate in 240 ml of dimethyl sulfoxide is stirred at 80° C. for 18 hours. After cooling, 400 ml of chloroform are added, and the mixture is extracted five times with 200 ml of water. The organic phase is dried over magnesium sulfate and the solvent is distilled off under reduced pressure. The residue is stirred with diethyl ether and dried under reduced pressure at 40° C.

후처리

  1. temperatureAfter cooling
  2. extractionthe mixture is extracted five times with 200 ml of water
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. distillationthe solvent is distilled off under reduced pressure
  5. stirringThe residue is stirred with diethyl ether
  6. customdried under reduced pressure at 40° C.

출처 및 근거

ORD 기록
ord-589c9b94c9d14b80be1d75ac0fa7a000
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07674825B2

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