Dimethylformamide → HCID 57974723, 화합물

HRID 1864723노트

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HRID 1864723 반응식
CN(C=O)C.[NH:6]1[CH:10]=[CH:9][N:8]=[C:7]1[C:11]1[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[Na+].[Na+].[N+:23]([C:26]1[CH:27]=[C:28]([CH:31]=[CH:32][CH:33]=1)[CH2:29]Cl)([O-:25])=[O:24]>O>[N+:23]([C:26]1[CH:27]=[C:28]([CH:31]=[CH:32][CH:33]=1)[CH2:29][N:6]1[CH:10]=[CH:9][N:8]=[C:7]1[C:11]1[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=1)([O-:25])=[O:24]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 10340Sodium CarbonateHCID 12078alpha-Chloro-m-nitrotolueneHCID 3168174-(1H-Imidazol-2-yl)-pyridine

생성물 1

HCID 57974723HCID 57974723, 화합물

시약·촉매·용매 1

HCID 962Water용매

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온도
50 °C

실험 절차

DMF (20 mL) is added to 4-(1H-Imidazol-2-yl)-pyridine (930 mg, 6.4 mmol), sodium carbonate (1.92 g, 20 mmol), and 3-nitrobenzyl chloride (1.71 g, 10 mmol) and the mixture is warmed to 50° C. for 4 h. Water (100 mL) is added and the corresponding mixture is extracted with EtOAc (100 mL), dried over anhydrous sodium sulfate, and crude solution is concentrated under reduced pressure. The organics are dissolved in DCM and filtered through a plug of silica eluting first with DCM, and then washing with 20% MeOH:80% DCM to afford 4-[1-(3-Nitro-benzyl)-1H-imidazol-2-yl]-pyridine as an off-white solid.

후처리

  1. extractionthe corresponding mixture is extracted with EtOAc (100 mL)
  2. dry with materialdried over anhydrous sodium sulfate, and crude solution
  3. concentrationis concentrated under reduced pressure
  4. dissolutionThe organics are dissolved in DCM
  5. filtrationfiltered through a plug of silica eluting first with DCM
  6. washwashing with 20% MeOH

출처 및 근거

ORD 기록
ord-8225807d2eca4f4dadf558460b50365f
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625931B2

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