2-Chloro-4-methoxypyrimidine → 4-methoxy-N-(4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)pyrimidin-2-amine

HRID 40729

反応式

HRID 40729 の反応式
Cl[C:2]1[N:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][C:11]1[N:15]=[CH:14][N:13]([C:16]2[CH:22]=[CH:21][C:19]([NH2:20])=[CH:18][CH:17]=2)[N:12]=1>C(OC(O)C)C.O.CCOC(C)=O>[CH3:9][O:8][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([NH:20][C:19]2[CH:18]=[CH:17][C:16]([N:13]3[CH:14]=[N:15][C:11]([CH3:10])=[N:12]3)=[CH:22][CH:21]=2)[N:7]=1

参加物

6

反応物 2

HCID 5889352-Chloro-4-methoxypyrimidineHCID 446274764-(3-Methyl-1H-1,2,4-triazol-1-yl)aniline

生成物 1

HCID 595881784-methoxy-N-(4-(3-methyl-1H-1,2,4-triazol-1-yl)phenyl)pyrimidin-2-amine

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒HCID 101298981-Ethoxyethanol溶媒

反応条件

温度
75 °C

実験手順

To a solution 2-chloro-4-methoxypyrimidine (2 g, 13.8 mmol) in ethoxyethanol (50 mL) was added 4-(3-methyl-1H-1,2,4-triazol-1-yl)aniline (1.7 g, 10.6 mmol). The reaction was warmed to 75° C. for 16 h, cooled, and diluted with water and EtOAc. The layers were separated, and the aqueous layer was extracted with EtOAc (4×). The combined organics were dried (MgSO4), and concentrated to give a near colorless solid which was homogeneous by analytical HPLC analysis and was used without further purification.

後処理

  1. temperaturecooled
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted with EtOAc (4×)
  4. dry with materialThe combined organics were dried (MgSO4)
  5. concentrationconcentrated
  6. customto give a near colorless solid which
  7. customwas used without further purification

出典と根拠

ORDレコード
ord-65f397ec3e8d46fcb30e760fe36cae26
出典データセット
uspto-grants-2013_09
特許番号
US08530480B2

関連ノート

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