Thiophenol → HCID 402511, 화합물

HRID 276974노트

반응식

HRID 276974 반응식
Cl[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][C:10](=[O:12])[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8][C:7]=2[CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[C:25]1([SH:31])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(O)C>[C:25]1([S:31][CH2:2][C:3]2[CH:4]=[CH:5][C:6]3[O:11][C:10](=[O:12])[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8][C:7]=3[CH:18]=2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

참가 물질

5

반응물 3

HCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 10659438Ethyl 6-chloromethyl-2-oxo-2H-1-benzopyran-3-carboxylate

생성물 1

HCID 402511HCID 402511, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1 g of ethyl 6-chloromethyl-2-oxo-2H-1-benzopyran-3-carboxylate (3.75 mmol), 0.57 g of potassium carbonate (4.13 mmol), 2.07 g of thiophenol (18.75 mmol) and 10 ml of absolute ethanol is reflux for 3 h. After removal of the solvent by distillation under reduced pressure, the residue is taken up in chloroform. The organic phase is washed with water and then dried over MgSO4. The solvent is removed by distillation under reduced pressure and the residue is washed with hexane to remove the excess thiophenol. The title product is recrystallized from ethyl acetate/petroleum ether.

후처리

  1. temperatureis reflux for 3 h
  2. customAfter removal of the solvent
  3. distillationby distillation under reduced pressure
  4. washThe organic phase is washed with water
  5. dry with materialdried over MgSO4
  6. customThe solvent is removed by distillation under reduced pressure
  7. washthe residue is washed with hexane
  8. customto remove the excess thiophenol
  9. customThe title product is recrystallized from ethyl acetate/petroleum ether

출처 및 근거

ORD 기록
ord-bc3cf4d6f6734b04aa103da6ccae100d
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355658B1

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