Potassium Phosphate, Tribasic → HCID 59477832、化合物

HRID 570846

反応式

HRID 570846 の反応式
[C:1]1([C:7]2[C:8]([C:12]#[N:13])=[CH:9][NH:10][CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:14]([O:16][C:17](=[O:25])[C:18]1[CH:23]=[CH:22][N:21]=[C:20](Br)[CH:19]=1)[CH3:15].P([O-])([O-])([O-])=O.[K+].[K+].[K+].CN[C@@H]1CCCC[C@H]1NC>C1(C)C=CC=CC=1.[Cu](I)I>[CH2:14]([O:16][C:17](=[O:25])[C:18]1[CH:19]=[CH:20][N:21]=[C:22]([N:10]2[CH:11]=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:8]([C:12]#[N:13])=[CH:9]2)[CH:23]=1)[CH3:15]

参加物

7

反応物 4

HCID 62657Potassium Phosphate, TribasicHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 37214604-Phenyl-1H-pyrrole-3-carbonitrileHCID 3847769Ethyl 2-bromoisonicotinate

生成物 1

HCID 59477832HCID 59477832、化合物収率 35%

試薬・触媒・溶媒 2

HCID 83717Copper iodide触媒HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

To a solution of 4-phenyl-1H-pyrrole-3-carbonitrile (0.1 g) in toluene (0.70 mL) were added 2-bromo-isonicotinic acid ethyl ester (0.19 g), potassium phosphate (0.31 g), (1R,2R)-(−)-N,N′-dimethylcyclohexane-1,2-diamine (0.02 g) and copper iodide (0.007 g) at room temperature, and this mixture was stirred at 110° C. for 24 hours. The insoluble material was removed by filtration through Celite, and this filtrate was concentrated. This obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/n-hexane=10/90-66/34) to give the title compound (0.066 g).

後処理

  1. customThe insoluble material was removed by filtration through Celite
  2. concentrationthis filtrate was concentrated
  3. customThis obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/n-hexane=10/90-66/34)

出典と根拠

ORDレコード
ord-fea73fa641114481b0084c1ccb5dd478
出典データセット
uspto-grants-2015_05
特許番号
US09023882B2

関連ノート

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