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Sodium Carbonate → 1-Phenyl-5-[3-(2,2,2-trifluoroethoxymethyl)phenyl]-1H-pyrazol-3-ylamine

HRID 83588
ノート
印刷プレビュー

反応式

HRID 83588 の反応式
I[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([NH2:13])[CH:3]=1.CC1(C)C(C)(C)OB([C:22]2[CH:27]=[CH:26][CH:25]=[C:24]([CH2:28][O:29][CH2:30][C:31]([F:34])([F:33])[F:32])[CH:23]=2)O1.C(=O)([O-])[O-].[Na+].[Na+].C1(P(C2CCCCC2)C2CCCCC2)CCCCC1.C(=O)([O-])O.[Na+]>COCCOC.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[C:7]1([N:6]2[C:2]([C:26]3[CH:27]=[CH:22][CH:23]=[C:24]([CH2:28][O:29][CH2:30][C:31]([F:32])([F:33])[F:34])[CH:25]=3)=[CH:3][C:4]([NH2:13])=[N:5]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 10340Sodium CarbonateHCID 75806TricyclohexylphosphineHCID 516892Sodium BicarbonateHCID 71287843HCID 71287843、化合物HCID 86680350HCID 86680350、化合物

生成物 1

HCID 712878771-Phenyl-5-[3-(2,2,2-trifluoroethoxymethyl)phenyl]-1H-pyrazol-3-ylamine収率 95.8%

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of 5-iodo-1-phenyl-1H-pyrazol-3-ylamine (221 mg) prepared according to the same procedures as Preparation 2 in 1,2-dimethoxyethane (2.2 ml) were sequentially added 4,4,5,5-tetramethyl-2-[3-(2,2,2-trifluoroethoxymethyl)phenyl]-[1,3,2]dioxaborolane (269 mg) prepared in Preparation 28, a 2M aqueous solution of sodium carbonate (1.1 ml), tricyclohexylphosphine (43.4 mg) and palladium (II) acetate (17.4 mg) at room temperature, and the mixture was stirred at 100° C. for 12 hours. To this reaction mixture was added a saturated aqueous solution of sodium hydrogen carbonate at room temperature, and then the mixture was filtered through Celite, and subjected to elution with ethyl acetate. The filtrate was extracted with ethyl acetate, the resulting organic layer was washed with was a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=2/1) to give the titled compound (258 mg).

後処理

  1. customprepared in Preparation 28
  2. filtrationthe mixture was filtered through Celite
  3. washsubjected to elution with ethyl acetate
  4. extractionThe filtrate was extracted with ethyl acetate
  5. washthe resulting organic layer was washed
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=2/1)

出典と根拠

ORDレコード
ord-82108d5c481947b389da4572ff719a22
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846746B2

反応ノート

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