Potassium Carbonate → 4-(Pyrimidin-5-yloxy)benzaldehyde

HRID 1926712노트

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HRID 1926712 반응식
[N:1]1[CH:6]=[C:5]([OH:7])[CH:4]=[N:3][CH:2]=1.F[C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=1.CS([O-])=O.[Na+].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[N:1]1[CH:6]=[C:5]([O:7][C:9]2[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=2)[CH:4]=[N:3][CH:2]=1

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 565855Pyrimidin-5-olHCID 2733271Sodium methanesulfinate

생성물 1

HCID 716702454-(Pyrimidin-5-yloxy)benzaldehyde수율 65.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

To a stirred solution of pyrimidin-5-ol (0.384 g, 4.0 mmol) in DMF (4.0 mL) were added 4-fluorobenzaldehyde (0.429 g, 4.0 mmol), sodium methanesulphinate (0.118 g, 1.0 mmol) and potassium carbonate (0.828 g, 6.0 mmol). The reaction mixture was heated at 120° C. for 3 hours, cooled to ambient temperature, treated with water and extracted three times with TBME. The extracts were washed with brine, dried and concentrated. Column chromatography gave 0.523 g (43%) of the subtitle compound.

후처리

  1. temperaturecooled to ambient temperature
  2. extractionextracted three times with TBME
  3. washThe extracts were washed with brine
  4. customdried
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-369e7e4fd3994e98b5bd82f8b6999eb9
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183251B2

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