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

HRID 373238노트

반응식

HRID 373238 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c446ae110285482c96bc7206d32408f3
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05162326

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