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Potassium Phosphate, Tribasic → 4'-Amino-5'-methoxy-N,2'-dimethylbiphenyl-4-carboxamide

HRID 2091950
ノート
印刷プレビュー

反応式

HRID 2091950 の反応式
Cl[C:2]1[C:8]([CH3:9])=[CH:7][C:5]([NH2:6])=[C:4]([O:10][CH3:11])[CH:3]=1.[CH3:12][NH:13][C:14]([C:16]1[CH:21]=[CH:20][C:19](B(O)O)=[CH:18][CH:17]=1)=[O:15].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1.[O-]P([O-])([O-])=O.[K+].[K+].[K+]>C(O)CCC.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[NH2:6][C:5]1[C:4]([O:10][CH3:11])=[CH:3][C:2]([C:19]2[CH:20]=[CH:21][C:16]([C:14]([NH:13][CH3:12])=[O:15])=[CH:17][CH:18]=2)=[C:8]([CH3:9])[CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 807824-Chloro-5-methyl-o-anisidineHCID 27735264-(Methylcarbamoyl)benzeneboronic acidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl

生成物 1

HCID 595867914'-Amino-5'-methoxy-N,2'-dimethylbiphenyl-4-carboxamide

試薬・触媒・溶媒 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 2631-Butanol溶媒

反応条件

温度
130 °C

実験手順

The mixture of 4-chloro-2-methoxy-5-methylaniline (2.0 g, 11.7 mmol), 4-(methylcarbamoyl)phenylboronic acid (2.08 g, 11.7 mmol), 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl (1.20 g, 2.9 mmol), Pd2(dba)3 (1.1 g, 1.2 mmol), and K3PO4 (7.4 g, 34.9 mmol) in 80 mL of n-butanol is degassed and heated at 130° C. overnight. The reaction mixture is filtered through a pad of celite, and concentrated in vacuo. The crude product mixture is partitioned between EtOAc and brine, the collected organic extracts are dried (Na2SO4), concentrated, and purified by silica gel chromatography (EtOAc/Hexanes:1/4) to afford 4′-Amino-5′-methoxy-N,2′-dimethylbiphenyl-4-carboxamide; ESMS m/z 271.1 (M+H+).

後処理

  1. customis degassed
  2. filtrationThe reaction mixture is filtered through a pad of celite
  3. concentrationconcentrated in vacuo
  4. customThe crude product mixture is partitioned between EtOAc and brine
  5. dry with materialthe collected organic extracts are dried (Na2SO4)
  6. concentrationconcentrated
  7. custompurified by silica gel chromatography (EtOAc/Hexanes:1/4)

出典と根拠

ORDレコード
ord-ea0f7abac9e943299b314cdd1ce31e0e
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08440681B2

反応ノート

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