Potassium Carbonate → HCID 58046337, 화합물

HRID 2359287

반응식

HRID 2359287 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([OH:12])[CH:5]=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9].C(=O)([O-])[O-].[K+].[K+].CC1C=CC([C:26]2[C:27]([F:37])=[C:28]([CH:32]=[C:33]([Cl:36])[C:34]=2F)[C:29]([O-:31])=[O:30])=CC=1>CS(C)=O>[Cl:36][C:33]1[C:34]([O:12][C:4]2[CH:5]=[CH:6][C:7]([C:8]([F:10])([F:11])[F:9])=[C:2]([Cl:1])[CH:3]=2)=[CH:26][C:27]([F:37])=[C:28]([CH:32]=1)[C:29]([O:31][C:4]1[CH:5]=[CH:6][C:7]([CH3:8])=[CH:2][CH:3]=1)=[O:30]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 136091473-Chloro-4-(trifluoromethyl)phenolHCID 866608804-Methylphenyl-5-chloro-2,4-difluorobenzoate

생성물 1

HCID 58046337HCID 58046337, 화합물수율 92.7%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of 3-chloro-4-(trifluoromethyl)phenol (Preparation 16, 100 mg, 0.470 mmol) in DMSO (1 mL) was added potassium carbonate (0.84 mg, 0.611 mmol) and the mixture stirred for 5 minutes. 4-methylphenyl-5-chloro-2,4-difluorobenzoate (Preparation 10, 0.133 mg, 0.470 mmol) was then added and the reaction stirred under nitrogen for 3 hours. The reaction was quenched by the addition of water (2 mL) and ethyl acetate (3 ml). The organic layer was separated, dried over magnesium sulfate and concentrated in vacuo to afford a white solid that was purified using silica gel column chromatography eluting with ethyl acetate:heptane 3:97 to furnish the title compound (100 mg, 47%).

후처리

  1. stirringthe reaction stirred under nitrogen for 3 hours
  2. customThe reaction was quenched by the addition of water (2 mL) and ethyl acetate (3 ml)
  3. customThe organic layer was separated
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customto afford a white solid
  7. customthat was purified
  8. washeluting with ethyl acetate:heptane 3:97

출처 및 근거

ORD 기록
ord-386b27ea5ec545df9c1bc582068ffebb
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685977B2

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