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Water → Methyl 2'-fluoro-5-(5-methylpyridin-2-yl)-6'-(trifluoromethyl)biphenyl-3-carboxylate

HRID 2278761
ノート
印刷プレビュー

反応式

HRID 2278761 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][CH3:14])=[O:12])=[N:6][CH:7]=1.Br[C:28]1[C:33]([C:34]([F:37])([F:36])[F:35])=[CH:32][CH:31]=[CH:30][C:29]=1[F:38].C(=O)([O-])[O-].[Cs+].[Cs+].O.CN(C)C=O>[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[F:38][C:29]1[CH:30]=[CH:31][CH:32]=[C:33]([C:34]([F:35])([F:36])[F:37])[C:28]=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]([O:13][CH3:14])=[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 5178472-Bromo-3-fluorobenzotrifluorideHCID 59432564Methyl 3-(5-methylpyridin-2-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate

生成物 1

HCID 67303854Methyl 2'-fluoro-5-(5-methylpyridin-2-yl)-6'-(trifluoromethyl)biphenyl-3-carboxylate

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 (300.0 mg, 0.8493 mmol), 2-bromo-1-fluoro-3-(trifluoromethyl)benzene (412.8 mg, 1.699 mmol), cesium carbonate (1384 mg, 4.247 mmol), tetra-n-butylammonium iodide (313.7 mg, 0.8493 mmol), and POPd (42.61 mg, 0.08493 mmol) were dissolved in Water (0.6 mL, 40 mmol) and N,N-dimethylformamide (3 mL, 40 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 (yellow oil) 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 (yellow oil)
  5. customused in the next reaction without further purification

出典と根拠

ORDレコード
ord-5c4152fa16cb4689ad68949adf930429
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

読み込み中…

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