Cesium carbonate → HCID 86586167, 화합물

HRID 433587노트

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HRID 433587 반응식
Cl[CH2:2][C:3]1[N:4]=[CH:5][N:6]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[C:10]([Cl:15])[CH:9]=2)[CH:7]=1.[NH:16]1[CH:20]=[CH:19][N:18]=[C:17]1[CH:21]=[O:22].C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C>[Cl:15][C:10]1[CH:9]=[C:8]([N:6]2[CH:7]=[C:3]([CH2:2][N:16]3[CH:20]=[CH:19][N:18]=[C:17]3[CH:21]=[O:22])[N:4]=[CH:5]2)[CH:13]=[CH:12][C:11]=1[Cl:14]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 249551H-imidazole-2-carbaldehydeHCID 234450324-Chloromethyl-1-(3,4-dichloro-phenyl)-1H-imidazole

생성물 1

HCID 86586167HCID 86586167, 화합물수율 61%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

4-Chloromethyl-1-(3,4-dichloro-phenyl)-1H-imidazole (1.31 g, 5.0 mmol) was dissolved in DMF (10 ml), 2-imidazolecarboxaldehyde (0.48 g, 5.0 mmol) and cesium carbonate (0.82 g, 2.5 mmol) was added and the resulting mixture was stirred at 60° C. for 12 h. After evaporation of the solvent the residue was dissolved in AcOEt and washed with H2O. The organic phase was dried (Na2SO4), concentrated and chromatographed [silica, elution with gradient CH2Cl2 to 100% (CH2Cl2/MeOH=9:1)] to obtain 0.98 g (61%) of the title compound as an off-white solid. Mp. 130-131° C. (CH2Cl2/iPr2O), MS: m/e=320 (M+).

후처리

  1. customAfter evaporation of the solvent the residue
  2. dissolutionwas dissolved in AcOEt
  3. washwashed with H2O
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. concentrationconcentrated
  6. customchromatographed
  7. wash[silica, elution with gradient CH2Cl2 to 100% (CH2Cl2/MeOH=9:1)]

출처 및 근거

ORD 기록
ord-ddadb30fbc9d4f52b3831f46ef27eae6
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06667335B2

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