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1,10-Phenanthroline → HCID 66893394, 화합물

HRID 1162002
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HRID 1162002 반응식
I[C:2]1[C:10]2[O:9][CH:8]=[CH:7][C:6]=2[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.[OH:14][CH2:15][CH2:16][N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1.C(=O)([O-])[O-].[Cs+].[Cs+].N1C2C(=CC=C3C=2N=CC=C3)C=CC=1>[Cu]I.C1(C)C=CC=CC=1>[N+:11]([C:4]1[CH:3]=[C:2]([O:14][CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[C:10]2[O:9][CH:8]=[CH:7][C:6]=2[CH:5]=1)([O-:13])=[O:12]
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참가 물질

7

반응물 4

HCID 13181,10-PhenanthrolineHCID 10796Cesium carbonateHCID 611632-MorpholinoethanolHCID 218647647-Iodo-5-nitrobenzofuran

생성물 1

HCID 66893394HCID 66893394, 화합물수율 32%

시약·촉매·용매 2

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 1140Toluene용매

실험 절차

To a test tube was added 7-iodo-5-nitrobenzofuran (1.0 g, 0.00346 mol), 4-(2-hydroxyethyl)morpholine (0.91 g, 0.00692 mol), cesium carbonate (2.25 g, 0.00692 mol), 1,10-phenanthroline (0.25 g, 0.00138 mol) and CuI (130 mg, 0.692 mmol). Toluene (15 mL) was added and the solution was heated in a StemBlock for 72 h. After filtration through Celite, the crude material was purified by flash chromatography (EtOAc/DCM; 1:1). Yield: 32%, HPLC purity=90%, m/z=293 (M+H)+.

후처리

  1. temperaturethe solution was heated in a StemBlock for 72 h
  2. filtrationAfter filtration through Celite
  3. customthe crude material was purified by flash chromatography (EtOAc/DCM; 1:1)

출처 및 근거

ORD 기록
ord-b51935799562419bb04cb2de739004f6
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07820675B2

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