Imidazole → HCID 68453232, 화합물

HRID 2356066노트

반응식

HRID 2356066 반응식
[I:1][C:2]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2.[Si:13](Cl)([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14].N1C=CN=C1.O>CN(C=O)C>[Si:13]([O:12][C:9]1[CH:10]=[CH:11][C:2]([I:1])=[C:3]2[C:8]=1[N:7]=[CH:6][CH:5]=[CH:4]2)([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14]

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 961115-Iodo-8-quinolinol

생성물 1

HCID 68453232HCID 68453232, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of Example 201A (10.40 g, 38.4 mmol), tert-butyldimethylsilyl chloride (6.07 g, 40.3 mmol), and imidazole (5.49 g, 80.6 mmol) in DMF (75 mL) at room temperature was stirred for 16 hours, treated with water (300 mL), and extracted with diethyl ether (3×400 mL). The combined extracts were washed with brine (100 mL), dried (Na2SO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 10% ethyl acetate/hexanes to provide the desired product.

후처리

  1. extractionextracted with diethyl ether (3×400 mL)
  2. washThe combined extracts were washed with brine (100 mL)
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe concentrate was purified by flash column chromatography on silica gel with 10% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-ffb772bef3f045c7b3bc80dc58661e26
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07754886B2

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