Sodium Acetate → HCID 68599246, 화합물

HRID 1185503노트

반응식

HRID 1185503 반응식
[CH2:1]([O:3][C:4](=[O:20])/[C:5](=[CH:12]/[C:13]1[CH:14]=[C:15]([CH3:19])[CH:16]=[CH:17][CH:18]=1)/[CH2:6][C:7]([O:9][CH2:10][CH3:11])=O)[CH3:2].C([O-])(=[O:23])C.[Na+]>C(OC(=O)C)(=O)C.O>[CH2:1]([O:3][C:4]([C:5]1[CH:6]=[C:7]([O:9][C:10](=[O:23])[CH3:11])[C:18]2[C:13](=[CH:14][C:15]([CH3:19])=[CH:16][CH:17]=2)[CH:12]=1)=[O:20])[CH3:2]

참가 물질

5

반응물 2

HCID 517045Sodium AcetateHCID 685999652-[1-m-Tolyl-meth-(e)-ylidene]-succinic acid diethyl ester

생성물 1

HCID 68599246HCID 68599246, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 7918Acetic Anhydride용매

실험 절차

To a solution of 2 g of 2-[1-m-Tolyl-meth-(E)-ylidene]-succinic acid diethyl ester in 10 ml of acetic acid anhydride, 594 mg sodium acetate was added and the reaction mixture was heated to reflux for 5 h. After cooling to RT the reaction mixture was diluted with water and extracted with ethyl acetate. The combined organic phases were washed three times with saturated aqueous sodium hydrogen carbonate solution. The organic phase was dried over MgSO4 and the solvents were removed under reduced pressure. The crude product was purified by chromatography on silica gel eluting with n-heptane/ethyl acetate (1/1). The fractions containing the product were combined and the solvent evaporated under reduced pressure. Yield: 860 mg.

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 5 h
  3. extractionextracted with ethyl acetate
  4. washThe combined organic phases were washed three times with saturated aqueous sodium hydrogen carbonate solution
  5. dry with materialThe organic phase was dried over MgSO4
  6. customthe solvents were removed under reduced pressure
  7. customThe crude product was purified by chromatography on silica gel eluting with n-heptane/ethyl acetate (1/1)
  8. additionThe fractions containing the product
  9. customthe solvent evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-3e1f709694944f8c88086839924f237f
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08669266B2

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