Potassium Phosphate, Tribasic → Methyl 6-methyl-2-phenyl-4-pyrimidinecarboxylate

HRID 553826

反応式

HRID 553826 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:10]=[C:9]([CH3:11])[N:8]=[C:7](Cl)[N:6]=1)=[O:4].[C:13]1(B(O)O)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].O.CC(=O)OCC>O1CCOCC1.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>[CH3:1][O:2][C:3]([C:5]1[CH:10]=[C:9]([CH3:11])[N:8]=[C:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:6]=1)=[O:4]

参加物

7

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 66827Phenylboronic AcidHCID 2736835Methyl 2-chloro-6-methylpyrimidine-4-carboxylateHCID 22728543Water ethylacetate

生成物 1

HCID 58101529Methyl 6-methyl-2-phenyl-4-pyrimidinecarboxylate

試薬・触媒・溶媒 2

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

実験手順

2-chloro-6-methyl-pyrimidine-4-carboxylic acid methyl ester (930 mg), phenylboronic acid (610 mg), tetrakis(triphenylphosphine)palladium (265 mg) and potassium phosphate (2.12 g) were dissolved in anhydrous dioxane (25 ml) under argon. The mixture was refluxed overnight and worked up with water/EA. The org. phases were dried (Na2SO4) and evaporated off. Column chromatography (EA/Hept 1/5) offered 875 mg of the desired compound.

後処理

  1. temperatureThe mixture was refluxed overnight
  2. dry with materialphases were dried (Na2SO4)
  3. customevaporated off

出典と根拠

ORDレコード
ord-99a308eb50b24b91a6980a55a346e494
出典データセット
uspto-grants-2011_11
特許番号
US08048881B2

関連ノート

読み込み中…