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Potassium Carbonate → HCID 44156374, 화합물

HRID 1628951
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HRID 1628951 반응식
C([O:4][CH:5]([C:8]1[C:13]2[N:14]3[CH2:20][CH2:19][CH2:18][N:17]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=4[Cl:28])[C:15]3=[N:16][C:12]=2[C:11]([Cl:29])=[CH:10][CH:9]=1)[CH2:6][CH3:7])(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:29][C:11]1[C:12]2[N:16]=[C:15]3[N:17]([C:21]4[CH:26]=[CH:25][C:24]([Cl:27])=[CH:23][C:22]=4[Cl:28])[CH2:18][CH2:19][CH2:20][N:14]3[C:13]=2[C:8]([CH:5]([OH:4])[CH2:6][CH3:7])=[CH:9][CH:10]=1
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참가 물질

4

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HCID 11430Potassium CarbonateHCID 441562551-[9-Chloro-1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]propyl acetate

생성물 1

HCID 44156374HCID 44156374, 화합물수율 71%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of (−)-1-[9-chloro-1-(2,4-dichlorophenyl)-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazol-6-yl]propyl acetate (79.6 mg, 0.176 mmol) in methanol (1.5 mL) was added potassium carbonate (36.4 mg, 0.264 mmol). The reaction mixture was stirred at room temperature for 1 hr. After the mixture was concentrated, the residue was diluted with water and extracted with ethyl acetate (×3). The combined organic layer was washed with brine (×1), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 0-50% ethyl acetate/n-hexane gradient mixture. The resulting solid was recrystallized from ethyl acetate/n-hexane to give the title compound as a colorless powder (51.1 mg, 0.124 mmol, 71%).

후처리

  1. concentrationAfter the mixture was concentrated
  2. additionthe residue was diluted with water
  3. extractionextracted with ethyl acetate (×3)
  4. washThe combined organic layer was washed with brine (×1)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by silica gel column chromatography
  9. washeluting with a 0-50% ethyl acetate/n-hexane gradient mixture
  10. customThe resulting solid was recrystallized from ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-d31db9b233b7468ca3dbb1221b2af367
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785460B2

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