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

HRID 40729

반응식

HRID 40729 반응식
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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 962Water용매HCID 8857Ethyl Acetate용매HCID 101298981-Ethoxyethanol용매

반응 조건

온도
75 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-65f397ec3e8d46fcb30e760fe36cae26
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530480B2

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