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Sodium Carbonate → 7-(4-Methoxy-2-methyl-phenyl)-2-methyl-2H-indazole

HRID 1350538
ノート
印刷プレビュー

反応式

HRID 1350538 の反応式
Br[C:2]1[C:10]2[C:6](=[CH:7][N:8]([CH3:11])[N:9]=2)[CH:5]=[CH:4][CH:3]=1.[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17](B(O)O)=[C:16]([CH3:23])[CH:15]=1.C(=O)([O-])[O-].[Na+].[Na+]>COCCOC.O.CCOC(C)=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:2]2[C:10]3[C:6](=[CH:7][N:8]([CH3:11])[N:9]=3)[CH:5]=[CH:4][CH:3]=2)=[C:16]([CH3:23])[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

8

反応物 3

HCID 10340Sodium CarbonateHCID 2773486(4-Methoxy-2-methylphenyl)boronic acidHCID 210945807-bromo-2-methyl-2H-indazole

生成物 1

HCID 210946097-(4-Methoxy-2-methyl-phenyl)-2-methyl-2H-indazole収率 91%

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒
HCID 962
Water
溶媒
HCID 80711,2-Dimethoxyethane溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

7-Bromo-2-methyl-2H-indazole (4; 1.76 g, 8.3 mMol) and tetrakis(triphenylphosphine)palladium(0) (0.28 g, 0.25 mMol) were stirred in 15 mL of DME under argon atmosphere for 30 min. 4-Methoxy-2-methylbenzeneboronic acid (1.52 g, 9.2 mMol) was added, immediately followed by a solution of sodium carbonate (3.1 g, 29.1 mMol) in 10 mL water. The mixture was heated at a gentle reflux for 4 hr, and then cooled to rt and diluted with EtOAc (150 mL). The organic phase was washed with brine and dried over magnesium sulfate. Evaporation of the solvent afforded an oil, which was flash chromatographed on SiO2 and eluted with hexane:EtOAc (9:1) to afford 4c (1.9 g; 91%).

後処理

  1. temperatureThe mixture was heated at
  2. temperaturea gentle reflux for 4 hr
  3. washThe organic phase was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customEvaporation of the solvent
  6. customafforded an oil, which
  7. customchromatographed on SiO2
  8. washeluted with hexane:EtOAc (9:1)

出典と根拠

ORDレコード
ord-7be26b18d67f4c43b88e305200aa304a
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07214699B2

反応ノート

読み込み中…

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