Potassium Carbonate → Methyl 5-(5-chloro-2-(((4'-chloro-[1,1'-biphenyl]-4-yl)(methyl)amino)methyl)phenyl)picolinate

HRID 405139ノート

反応式

HRID 405139 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][C:4]=1[C:10]1[CH:11]=[CH:12][C:13]([C:16]([O:18][CH3:19])=[O:17])=[N:14][CH:15]=1.[Cl:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:32]=[CH:31][C:30]([NH:33][CH3:34])=[CH:29][CH:28]=2)=[CH:23][CH:22]=1.C([O-])([O-])=O.[K+].[K+]>CC(C)=O.CCOC(C)=O>[Cl:9][C:6]1[CH:7]=[CH:8][C:3]([CH2:2][N:33]([C:30]2[CH:29]=[CH:28][C:27]([C:24]3[CH:25]=[CH:26][C:21]([Cl:20])=[CH:22][CH:23]=3)=[CH:32][CH:31]=2)[CH3:34])=[C:4]([C:10]2[CH:11]=[CH:12][C:13]([C:16]([O:18][CH3:19])=[O:17])=[N:14][CH:15]=2)[CH:5]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 156227444-(4-Chlorophenyl)-N-methylanilineHCID 86674247Methyl 5-(2-(bromomethyl)-5-chlorophenyl)picolinate

生成物 1

HCID 71059984Methyl 5-(5-chloro-2-(((4'-chloro-[1,1'-biphenyl]-4-yl)(methyl)amino)methyl)phenyl)picolinate

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

Methyl 5-(2-(bromomethyl)-5-chlorophenyl)picolinate (200 mg, 0.59 mmol), 4′-chloro-N-methyl-[1,1′-biphenyl]-4-amine (141 mg, 0.65 mmol), and K2CO3 (122 mg, 0.88 mmol) were diluted with acetone (3 mL) and heated to 50° C. After 18 h the resulting mixture was diluted with EtOAc, washed with water and brine, dried (Na2SO4), and dry packed onto silica gel. Column chromatography yielded the title compound.

後処理

  1. washwashed with water and brine
  2. dry with materialdried (Na2SO4)
  3. customdry

出典と根拠

ORDレコード
ord-55d02b368df94ed48396974f2a5eab8b
出典データセット
uspto-grants-2014_06
特許番号
US08748624B2

反応ノート

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