Potassium Carbonate → HCID 86700048、化合物

HRID 1428098ノート

反応式

HRID 1428098 の反応式
[Br:1][C:2]1[C:3]([NH2:9])=[N:4][CH:5]=[C:6](I)[CH:7]=1.[CH3:10][O:11][C:12]1[CH:13]=[C:14](B(O)O)[CH:15]=[CH:16][C:17]=1[O:18][CH3:19].C(=O)([O-])[O-].[K+].[K+].[Cl-].[NH4+]>O1CCOCC1.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>[Br:1][C:2]1[C:3]([NH2:9])=[N:4][CH:5]=[C:6]([C:15]2[CH:14]=[CH:13][C:12]([O:11][CH3:10])=[C:17]([O:18][CH3:19])[CH:16]=2)[CH:7]=1

参加物

8

反応物 4

HCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 27347023,4-Dimethoxyphenylboronic acidHCID 176094413-Bromo-5-iodopyridin-2-amine

生成物 1

HCID 86700048HCID 86700048、化合物収率 94.9%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

3-Bromo-5-iodopyridin-2-amine (7.50 g), 3,4-dimethoxyphenylboronic acid (4.79 g), tetrakis(triphenylphosphine)palladium (1.45 g) and potassium carbonate (10.4 g) were suspended in dioxane (100 ml) and water (10 ml), and the suspension was heated at 80° C. for 9.5 hours. After leaving to cool, a saturated aqueous ammonium chloride solution was added, and the organic layer was extracted with ethyl acetate and dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [ethyl acetate] to give 7.36 g of the title compound as a solid.

後処理

  1. customAfter leaving
  2. temperatureto cool
  3. extractionthe organic layer was extracted with ethyl acetate
  4. dry with materialdried over sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe residue was purified by silica gel column chromatography [ethyl acetate]

出典と根拠

ORDレコード
ord-a53daad04b8b4a6090092417a66ae3e6
出典データセット
uspto-grants-2015_01
特許番号
US08933103B2

反応ノート

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