Cesium carbonate → HCID 58577309, 화합물

HRID 82561

반응식

HRID 82561 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([N:10]3[C:14]4=[N:15][CH:16]=[CH:17][CH:18]=[C:13]4[N:12]([CH2:19][CH3:20])[C:11]3=[O:21])=[CH:7][CH:8]=2)[CH2:3][CH2:2]1.Cl[C:23]1[S:24][CH:25]=[CH:26][N:27]=1.C([O-])([O-])=O.[Cs+].[Cs+].C([O-])(O)=O.[Na+]>CN(C=O)C>[CH2:19]([N:12]1[C:13]2[C:14](=[N:15][CH:16]=[CH:17][CH:18]=2)[N:10]([C:6]2[CH:5]=[C:4]3[C:9](=[CH:8][CH:7]=2)[N:1]([C:23]2[S:24][CH:25]=[CH:26][N:27]=2)[CH:2]=[CH:3]3)[C:11]1=[O:21])[CH3:20]

참가 물질

6

반응물 4

HCID 10796Cesium carbonateHCID 764292-ChlorothiazoleHCID 516892Sodium BicarbonateHCID 585772823-(2,3-dihydro-1H-indol-5-yl)-1-ethyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one

생성물 1

HCID 58577309HCID 58577309, 화합물수율 27.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 3-(2,3-dihydro-1H-indol-5-yl)-1-ethyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (75 mg), 2-chlorothiazole (48.0 mg) and Cs2CO3 (174 mg) in DMF (3 mL) was stirred at 100° C. for 3 days, treated with saturated NaHCO3 solution, and extracted with AcOEt. The organic layer was separated, dried over MgSO4 and concentrated in vacuo. The residue was purified by prep. HPLC and crystallized from AcOEt/Hexane to give the title compound as white crystals (27.0 mg).

후처리

  1. extractionextracted with AcOEt
  2. customThe organic layer was separated
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by prep
  6. customHPLC and crystallized from AcOEt/Hexane

출처 및 근거

ORD 기록
ord-a616ade2b40049af96929bb3f057c80d
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846713B2

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