Potassium Carbonate → 6-chloro-1-(2'-cyanobiphenyl-4-yl)methyl-3-propylpyrimidine-2,4(1H,3H)-dione

HRID 373238ノート

反応式

HRID 373238 の反応式
[Cl:1][C:2]1[NH:7][C:6](=[O:8])[N:5]([CH2:9][CH2:10][CH3:11])[C:4](=[O:12])[CH:3]=1.Cl[CH2:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:27]#[N:28])=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[N:7]([CH2:14][C:15]2[CH:16]=[CH:17][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]#[N:28])=[CH:19][CH:20]=2)[C:6](=[O:8])[N:5]([CH2:9][CH2:10][CH3:11])[C:4](=[O:12])[CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 6408466-chloro-3-propylpyrimidine-2,4(1H,3H)-dioneHCID 217117564'-(chloromethyl)-[1,1'-Biphenyl]-2-carbonitrile

生成物 1

HCID 198115376-chloro-1-(2'-cyanobiphenyl-4-yl)methyl-3-propylpyrimidine-2,4(1H,3H)-dione収率 98%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 6-chloro-3-propylpyrimidine-2,4(1H,3H)-dione (3 g), 4-chloromethyl-2'-cyanobiphenyl (4.76 g) and potassium carbonate (2.64 g) in DMF (50 ml) was stirred at room temperature for 3 hours and then at 60° C. for 2 hours. The reaction mixture was concentrated to dryness in vacuo and then the residue was dissolved in methylene chloride. The insoluble material was removed from the reaction mixture by filtration and the filtrate was concentrated to dryness. The resulting residue was purified by column chromatography on silica gel to give colorless crystals (5.9 g, 98%).

後処理

  1. waitat 60° C. for 2 hours
  2. concentrationThe reaction mixture was concentrated to dryness in vacuo
  3. dissolutionthe residue was dissolved in methylene chloride
  4. customThe insoluble material was removed from the reaction mixture by filtration
  5. concentrationthe filtrate was concentrated to dryness
  6. customThe resulting residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-c446ae110285482c96bc7206d32408f3
出典データセット
uspto-grants-1992_11
特許番号
US05162326

反応ノート

読み込み中…