Furan → 2-(4-Methoxycarbonylbutyryl)furan

HRID 1194130

반응식

HRID 1194130 반응식
C[CH:2]([CH2:7][C:8]([OH:10])=[O:9])[CH2:3][C:4]([OH:6])=O.[O:11]1[CH:15]=[CH:14][CH:13]=[CH:12]1.Cl[CH:17](Cl)C(OC(=O)C(Cl)Cl)=O>C1(C)C=CC=CC=1>[CH3:17][O:10][C:8]([CH2:7][CH2:2][CH2:3][C:4]([C:12]1[O:11][CH:15]=[CH:14][CH:13]=1)=[O:6])=[O:9]

참가 물질

5

반응물 3

HCID 8029FuranHCID 122843-Methylglutaric acidHCID 77772Acetic acid, 2,2-dichloro-, 1,1'-anhydride

생성물 1

HCID 138151342-(4-Methoxycarbonylbutyryl)furan수율 97.2%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
50 °C

실험 절차

In 50 ml of toluene were dissolved 7.31 g (0.05 mole) of monomethylglutaric acid, 4.43 g (0.085 mole) of furan and 14.39 g (0.06 mole) of dichloroacetic anhydride. To the resulting solution was added 0.71 g of boron trifluoride-diethyl ether complex and the resulting mixture was then stirred at 50° C. for 3 hours. After completion of the reaction, the reaction solution was cooled and washed successively with 5% aqueous sodium carbonate solution and water. The organic layer was concentrated under reduced pressure and the resulting concentrated residue was then purified by silica gel-filled column chromatography to obtain 9.54 g of 2-(4-methoxycarbonylbutyryl)furan.

후처리

  1. additionTo the resulting solution was added 0.71 g of boron trifluoride-diethyl ether complex
  2. customAfter completion of the reaction
  3. temperaturethe reaction solution was cooled
  4. washwashed successively with 5% aqueous sodium carbonate solution and water
  5. concentrationThe organic layer was concentrated under reduced pressure
  6. customthe resulting concentrated residue was then purified by silica gel-
  7. additionfilled column chromatography

출처 및 근거

ORD 기록
ord-bc85d02c97ed4ca384c3fcf7c2e4cd90
출처 데이터셋
uspto-grants-1989_03
특허 번호
US04812585

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