Potassium Carbonate → 3'-fluoro-4'-[(4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl)methyl]biphenyl-2-carbonitrile

HRID 1718981ノート

反応式

HRID 1718981 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([CH2:8][CH2:9][CH3:10])[NH:5][C:4](=[O:11])[CH:3]=1.Br[CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[C:21]([C:26]#[N:27])=[CH:22][CH:23]=[CH:24][CH:25]=2)=[CH:16][C:15]=1[F:28].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[F:28][C:15]1[CH:16]=[C:17]([C:20]2[C:21]([C:26]#[N:27])=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:18]=[CH:19][C:14]=1[CH2:13][N:5]1[C:4](=[O:11])[CH:3]=[C:2]([CH3:1])[N:7]=[C:6]1[CH2:8][CH2:9][CH3:10]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 574600744'-(Bromomethyl)-3'-fluorobiphenyl-2-carbonitrileHCID 1355166076-methyl-2-propylpyrimidin-4(3H)-one

生成物 1

HCID 574609673'-fluoro-4'-[(4-methyl-6-oxo-2-propylpyrimidin-1(6H)-yl)methyl]biphenyl-2-carbonitrile収率 29.5%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
50 °C

実験手順

To a solution of 6-methyl-2-propylpyrimidin-4(3H)-one (2.0 g) and 4′-(bromomethyl)-3′-fluorobiphenyl-2-carbonitrile (4.4 g) in acetonitrile (50 mL) was added potassium carbonate (3.6 g), and the mixture was stirred at 50° C. for 12 hr. The insoluble material was filtered off, the filtrate was concentrated, and the residue was purified by silica gel column chromatography to give the title compound (1.4 g, 29%) as a colorless viscous substance.

後処理

  1. filtrationThe insoluble material was filtered off
  2. concentrationthe filtrate was concentrated
  3. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-371cd305ea904157913a280082de5099
出典データセット
uspto-grants-2010_09
特許番号
US07803940B2

反応ノート

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