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Phenyl dihydrogen orthoborate → HCID 57514566、化合物

HRID 1182915
ノート
印刷プレビュー

反応式

HRID 1182915 の反応式
Br[C:2]1[CH:11]=[C:10]([CH3:12])[CH:9]=[C:8]2[C:3]=1[N:4]=[CH:5][CH:6]=[N:7]2.[C:13]1(OB(O)O)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>O1CCOCC1.CO.C(=O)([O-])[O-].[Na+].[Na+].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][C:10]1[CH:9]=[C:8]2[C:3]([N:4]=[CH:5][CH:6]=[N:7]2)=[C:2]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:11]=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 2

HCID 78412Phenyl dihydrogen orthoborateHCID 451174635-Bromo-7-methylquinoxaline

生成物 1

HCID 57514566HCID 57514566、化合物

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒HCID 887Methanol溶媒HCID 10340Sodium Carbonate
溶媒
HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 400 mg of 5-bromo-7-methyl-quinoxaline, 244 mg of phenylboric acid and 100 mg of tetrakis(triphenylphosphine)palladium in 12 ml dioxane, 4 ml of methanol and 3.6 ml 1 M aqueous sodium carbonate solution is refluxed for three hours under an argon atmosphere. Then the reaction mixture is evaporated down and the residue is distributed between ethyl acetate and water. The ethyl acetate phase is separated off, dried over magnesium sulphate and evaporated down. The crude product is purified by chromatography over a silica gel column with cyclohexane/ethyl acetate (85:15 to 70:30) as eluant.

後処理

  1. temperatureis refluxed for three hours under an argon atmosphere
  2. customThen the reaction mixture is evaporated down
  3. customThe ethyl acetate phase is separated off
  4. dry with materialdried over magnesium sulphate
  5. customevaporated down
  6. customThe crude product is purified by chromatography over a silica gel column with cyclohexane/ethyl acetate (85:15 to 70:30) as eluant

出典と根拠

ORDレコード
ord-a9a18cfe52454756a7b8e9d13f6f397f
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08664232B2

反応ノート

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