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Water → 2',3'-Difluoro-5-(5-methylpyridin-2-yl)biphenyl-3-carboxylic acid

HRID 2278756
ノート
印刷プレビュー

反応式

HRID 2278756 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[C:10]([CH:15]=[C:16](B3OC(C)(C)C(C)(C)O3)[CH:17]=2)[C:11]([O:13]C)=[O:12])=[N:6][CH:7]=1.Br[C:28]1[CH:33]=[CH:32][CH:31]=[C:30]([F:34])[C:29]=1[F:35].C(=O)([O-])[O-].[Cs+].[Cs+].O.CN(C)C=O>[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[F:34][C:30]1[C:29]([F:35])=[CH:28][CH:33]=[CH:32][C:31]=1[C:16]1[CH:17]=[C:8]([C:5]2[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][N:6]=2)[CH:9]=[C:10]([C:11]([OH:13])=[O:12])[CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 962WaterHCID 6228DimethylformamideHCID 10796Cesium carbonateHCID 27332601-Bromo-2,3-difluorobenzeneHCID 59432564Methyl 3-(5-methylpyridin-2-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate

生成物 1

HCID 584493602',3'-Difluoro-5-(5-methylpyridin-2-yl)biphenyl-3-carboxylic acid

試薬・触媒・溶媒 1

HCID 67553Tetrabutylammonium Iodide触媒

実験手順

In a 5 mL microwave vial, methyl 3-(5-methylpyridin-2-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (250 mg, 0.71 mmol), 1-bromo-2,3-difluorobenzene (273.2 mg, 1.416 mmol), cesium carbonate (1153 mg, 3.539 mmol), tetra-n-butylammonium iodide (261.4 mg, 0.7078 mmol), and POPd (35.51 mg, 0.07078 mmol) were dissolved in Water (0.5 mL, 30 mmol) and N,N-dimethylformamide (3 mL, 30 mmol). The reaction mixture was microwaved for 10 mins at 150 degrees. The reaction mixture was extracted with ethylacetate and washed repeatedly with brine. The solvent removed under reduced pressure and used in the next reaction without further purification.

後処理

  1. customThe reaction mixture was microwaved for 10 mins at 150 degrees
  2. extractionThe reaction mixture was extracted with ethylacetate
  3. washwashed repeatedly with brine
  4. customThe solvent removed under reduced pressure
  5. customused in the next reaction without further purification

出典と根拠

ORDレコード
ord-328ed60727c445bc99ed83a823ba5d37
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133122B2

反応ノート

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