Potassium Carbonate → HCID 86679897、化合物

HRID 81504

反応式

HRID 81504 の反応式
C(=O)([O-])[O-].[K+].[K+].[F:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[OH:15].CS([C:20]1[N:21]=[C:22]([O:46][CH2:47][CH2:48][CH3:49])[C:23]2[N:28]=[C:27]([C:29]3[CH:43]=[C:42]([CH3:44])[C:32]([O:33][CH2:34][C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])=[C:31]([CH3:45])[CH:30]=3)[O:26][C:24]=2[N:25]=1)(=O)=O.S(=O)(=O)(O)[O-].[Na+]>CN(C)C=O.O>[F:7][C:8]1[CH:13]=[CH:12][C:11]([F:14])=[CH:10][C:9]=1[O:15][C:20]1[N:21]=[C:22]([O:46][CH2:47][CH2:48][CH3:49])[C:23]2[N:28]=[C:27]([C:29]3[CH:30]=[C:31]([CH3:45])[C:32]([O:33][CH2:34][C:35]([O:37][C:38]([CH3:39])([CH3:40])[CH3:41])=[O:36])=[C:42]([CH3:44])[CH:43]=3)[O:26][C:24]=2[N:25]=1

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 949522,5-DifluorophenolHCID 516919Sodium BisulfateHCID 86679896HCID 86679896、化合物

生成物 1

HCID 86679897HCID 86679897、化合物収率 62.6%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

62 mg of potassium carbonate and 32 mg of 2,5-difluorophenol were added to a solution of 100 mg of tert-butyl [4-(5-methanesulfonyl-7-propoxyoxazolo[5,4-d]pyrimidin-2-yl)-2,6-dimethylphenoxy]acetate in 1.5 ml of N,N-dimethylformamide. The mixture was stirred at room temperature for 12 h. The mixture was then poured into water, neutralized by addition of 10% strength aqueous sodium bisulfate solution and extracted twice with ethyl acetate. The combined organic layers were dried and concentrated under reduced pressure. After filtration, the solvent was distilled off under reduced pressure and the residue was purified by preparative HPLC, giving 69 mg of the title compound.

後処理

  1. extractionextracted twice with ethyl acetate
  2. customThe combined organic layers were dried
  3. concentrationconcentrated under reduced pressure
  4. filtrationAfter filtration
  5. distillationthe solvent was distilled off under reduced pressure
  6. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-08030952854146e0b67b9d3d8884cd4d
出典データセット
uspto-grants-2014_09
特許番号
US08846691B2

関連ノート

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