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Potassium Carbonate → HCID 21082088, 화합물

HRID 347014
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HRID 347014 반응식
[Br-].[NH2:2][C:3]1[CH:12]=[C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([CH:20]([C:27]3[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][CH:28]=3)[C:21]3[N:25]([CH3:26])[CH:24]=[N:23][N:22]=3)[CH:9]=2)[N+:4]=1[CH2:34][C:35](=O)[C:36]([O:38][CH2:39][CH3:40])=[O:37].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[Cl:19][C:15]1[CH:14]=[C:13]([C:11]2[C:10]3[C:5](=[CH:6][CH:7]=[C:8]([CH:20]([C:27]4[CH:28]=[CH:29][C:30]([Cl:33])=[CH:31][CH:32]=4)[C:21]4[N:25]([CH3:26])[CH:24]=[N:23][N:22]=4)[CH:9]=3)[N:4]3[CH:34]=[C:35]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[N:2]=[C:3]3[CH:12]=2)[CH:18]=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 21082014HCID 21082014, 화합물

생성물 1

HCID 21082088HCID 21082088, 화합물수율 27.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of intermediate (67) (0.0006 mol), obtained in Example A12 g, in ethanol (3 ml) was stirred and refluxed for 18 hours. Potassium carbonate 10% was added. The mixture was extracted with DCM. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated till dryness. The residue (0.3 g) was purified by column chromatography over kromasil (eluent: CH2Cl2 100 to CH2Cl2/CH3OH 90/10; 10 μm). The pure fractions were collected and the solvent was evaporated. The residue (0.12 g, 33%) was crystallized from CH3CN/DIPE. The precipitate was filtered off and dried, yielding 0.091 g (25%) of ethyl 5-(3-chlorophenyl)-7-[(4-chlorophenyl)(4-methyl-4H-1,2,4-triazol-3-yl)methyl]-imidazo[1,2-a]quinoline-2-carboxylate, mp. 220° C.

후처리

  1. temperaturerefluxed for 18 hours
  2. extractionThe mixture was extracted with DCM
  3. customThe organic layer was separated
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was evaporated till dryness
  7. customThe residue (0.3 g) was purified by column chromatography over kromasil (eluent: CH2Cl2 100 to CH2Cl2/CH3OH 90/10; 10 μm)
  8. customThe pure fractions were collected
  9. customthe solvent was evaporated
  10. customThe residue (0.12 g, 33%) was crystallized from CH3CN/DIPE
  11. filtrationThe precipitate was filtered off
  12. customdried

출처 및 근거

ORD 기록
ord-3bdfe5cbd3874f77b8e535fff902f503
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07173040B2

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